CN102464524A - Method for producing low-carbon olefins from methanol - Google Patents
Method for producing low-carbon olefins from methanol Download PDFInfo
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- CN102464524A CN102464524A CN2010105523888A CN201010552388A CN102464524A CN 102464524 A CN102464524 A CN 102464524A CN 2010105523888 A CN2010105523888 A CN 2010105523888A CN 201010552388 A CN201010552388 A CN 201010552388A CN 102464524 A CN102464524 A CN 102464524A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a method for producing low-carbon olefins from methanol, which mainly solves the problem of lower yield of the low-carbon olefins in the prior art. According to the technical scheme provided by the invention, the method comprises the following steps: (a) a first raw material is in contact with a molecular sieve catalyst in a fluidized bed reactor, a product material flow I which comprises the low-carbon olefins is produced, and meanwhile, a carbon deposition catalyst is formed, wherein the first raw material mainly comprises the methanol; (b) the carbon deposition catalyst enters a regenerator for regeneration through a spent sloped tube, so that a regenerated catalyst is formed; and (c) one part of the regenerated catalyst returns to a position of 1/5-2/3 of a reaction zone of the fluidized bed reactor through the spent sloped tube, the other part of the regenerated catalyst enters a lift pipe to be in contact with a second raw material, a product material flow II which comprises the low-carbon olefins is produced, and the catalyst is carried into a deposition zone of the fluidized bed reactor. With the adoption of the technical scheme, the problem is better solved, so that the method can be applied to the industrial production of the low-carbon olefins.
Description
Technical field
The present invention relates to a kind of method of preparing low carbon olefin hydrocarbon with methanol.
Technical background
Low-carbon alkene, promptly 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 through petroleum path, but because limited supply of petroleum resources and higher price, 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 system ethene, propylene.Wherein, One type of important alternative materials that is used for low-carbon alkene production is an oxygenatedchemicals; For example alcohols (methyl alcohol, ethanol), ethers (dme, methyl ethyl ether), ester class (methylcarbonate, methyl-formiate) etc., these oxygenatedchemicalss can be transformed through coal, Sweet natural gas, biomass equal energy source.Some oxygenatedchemicals can reach fairly large production, like methyl alcohol, can be made by coal or Sweet natural gas, and technology is very ripe, can realize up to a million tonnes industrial scale.Because the popularity in oxygenatedchemicals source is added and is transformed the economy that generates low-carbon alkene technology, so by the technology of oxygen-containing compound conversion to produce olefine (OTO), particularly the technology by methanol conversion system alkene (MTO) receives increasing attention.
In US 4499327 patents silicoaluminophosphamolecular molecular sieves catalyst applications is studied in great detail in methanol conversion system olefin process, think that SAPO-34 is the first-selected catalyzer of MTO technology.The SAPO-34 catalyzer has very high selectivity of light olefin, and activity is also higher, and can make methanol conversion is the degree that was less than in reaction times of low-carbon alkene 10 seconds, more even reach in the reaction time range of riser tube.
Announced among the US 6166282 that a kind of methanol conversion is the technology and the reactor drum of low-carbon alkene; Adopt fast fluidized bed reactor; Gas phase is after the lower Mi Xiangfanyingqu reaction of gas speed is accomplished; 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 significantly reduce.But yield of light olefins is general all about 77% in this method, has the lower problem of yield of light olefins.
Announced among the CN 1723262 that it is low-carbon alkene technology that the multiple riser reaction unit that has central catalyst return is used 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 product gas are separated.Yield of light olefins is general all between 75～80% in this method, has the lower problem of yield of light olefins equally.
Known in the field; Prepare in the process of low-carbon alkene at methyl alcohol; Inevitably can produce by products such as carbon four above hydrocarbon; The utilization again of this part by product will be directly connected to the economy of whole methanol-to-olefins technology, and prior art does not still address this problem preferably, all has the lower problem of yield of light olefins.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 yield of light olefins that exists in the prior art, and a kind of method of new preparing low carbon olefin hydrocarbon with methanol is provided.This method is used for the production of low-carbon alkene, has the yield of light olefins advantage of higher.
For addressing the above problem; The technical scheme that the present invention adopts is following: a kind of method of preparing low carbon olefin hydrocarbon with methanol; Said method comprising the steps of: first raw material that (a) is mainly methyl alcohol contacts with sieve catalyst in fluidized-bed reactor; Generation comprises the product stream I of low-carbon alkene, forms carbon deposition catalyst simultaneously; (b) said carbon deposition catalyst gets into revivifier regeneration through inclined tube to be generated, forms regenerated catalyst; (c) a said regenerated catalyst part is returned 1/5～2/3 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube; A part gets into riser tube; Contact with second raw material, generate the product stream II that comprises low-carbon alkene, carry catalyzer and get into said fluidized-bed reactor negative area.
In the technique scheme, at least a in SAPO-18, SAPO-34 of said molecular screening, preferred version is SAPO-34; Said fluidized-bed reactor is a fast fluidized bed; Said regenerated catalyst gets into riser tube after outgasing, riser tube is built in the revivifier, and degas zone is built in the revivifier; Said second raw material is the alkene of carbon four～carbon six; Said riser tube quantity is at least 1; The shared cover separation process of said product stream I and product stream II; Reaction conditions is in the said fluidized-bed reactor: temperature of reaction is 400～500 ℃, and the gas phase linear speed is 0.8～2.0 meter per second, and the regenerator sloped tube mass flow of catalyst is 0.6～2.0: 1 with the ratio of the mass rate of first raw material; Reaction conditions is in the said riser tube: temperature of reaction is 550～650 ℃, and the gas phase linear speed is 5～10 meter per seconds; Said regenerated catalyst 20～50% returns 1/3～2/3 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube, and 50-80% gets into riser tube.
The carbon four above hydrocarbon by products that second raw material according to the invention obtains from centrifugal station, the alkene mass content is greater than 60%.
The all right non-imposed a certain proportion of thinner co-fed of interpolation in reactor feed; Thinner can be low-carbon alkanes (methane, ethane), CO, nitrogen, water vapour, C4 hydrocarbon, mononuclear aromatics etc.; Wherein, Preferred low-carbon alkanes, water vapour, most preferably scheme is a water vapour, the amount of thinner and the volume ratio of raw material are 0.1～10: regulate in 1 scope.
The preparation method of the silicoaluminophosphamolecular molecular sieve that the present invention adopted 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): 2～500 H
2O, wherein R represents template, and the constitutive material mixed solution obtains through after the crystallization of certain hour at a certain temperature; Once more, with molecular sieve presoma, phosphorus source, silicon source, aluminium source, organic formwork agent, water etc. according to after at least 0.1 hour, finally obtaining the SAPO molecular sieve at 110～260 ℃ of following hydrothermal crystallizings after certain mixed.
The molecular sieve of preparation is mixed with a certain proportion of sticker, and through obtaining final SAPO catalyzer after the operation stepss such as spraying drying, roasting, the weight percentage of sticker in molecular sieve is generally between 10～90%.
In methanol-to-olefins reaction process, can produce by products such as carbon four above hydrocarbon, wherein the olefin(e) centent in the carbon four above hydrocarbon is very high, under appropriate condition, can further be converted into low-carbon alkenes such as ethene, propylene fully.Adopt method of the present invention, at least one riser tube is set, be used to transform carbon four above hydrocarbon, improved yield of light olefins.In addition, regenerated catalyst returns 1/5～2/3 place of fluidized-bed reactor reaction zone among the present invention, can play the purpose that improves selectivity of light olefin, further improves yield of light olefins.
Adopt technical scheme of the present invention: at least a in SAPO-18, SAPO-34 of said molecular screening; Said fluidized-bed reactor is a fast fluidized bed; Said regenerated catalyst gets into riser tube after outgasing, riser tube is built in the revivifier, and degas zone is built in the revivifier; Said second raw material is the alkene of carbon four～carbon six; Said riser tube quantity is at least 1; The shared cover separation process of said product stream I and product stream II; Reaction conditions is in the said fluidized-bed reactor: temperature of reaction is 400～500 ℃, and the gas phase linear speed is 0.8～2.0 meter per second, and the regenerator sloped tube mass flow of catalyst is 0.6～2.0: 1 with the ratio of the mass rate of first raw material; Reaction conditions is in the said riser tube: temperature of reaction is 550～650 ℃, and the gas phase linear speed is 5～10 meter per seconds; Said regenerated catalyst 20～50% returns 1/3～2/3 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube; 50～80% get into riser tube; Low-carbon alkene carbon back yield can reach 89.13% weight; Low-carbon alkene carbon back yield increase rate than prior art can reach 9 percentage points, has obtained better technical effect.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
Among Fig. 1,1 is the first raw material charging; 2 is reactor reaction zone; 3 are gas-solid sharp separation equipment; 4 is stripping zone; 5 is reclaimable catalyst circulation inclined tube; 6 is inclined tube to be generated; 7 is interchanger; 8 is the reactor drum gas-solid cyclone separator; 9 is the reactor drum negative area; 10 is the product collection chamber; 11 is the product stream outlet line; 12 is regenerator sloped tube; 13 is the revivifier gas-solid cyclone separator; 14 is the regenerating medium source line; 15 are degassing medium inlet pipeline; 16 is the second material feeding tube line; 17 is degas zone; 18 is the revivifier breeding blanket; 19 is the revivifier negative area; 20 is riser tube; 21 is the regenerated flue gas outlet line; 22 is gas-solid cyclone separator.
First raw material gets in the reactor reaction zone 2 through feeding line 1; Contact with sieve catalyst; Reaction generates the product that contains low-carbon alkene, carries reclaimable catalyst and gets into reactor drum negative area 9 through gas-solid sharp separation equipment 3, wherein; Most of catalyzer that gas-solid sharp separation equipment 3 is separated gets into stripping zone 4; And gaseous products and part are not separated through going into cyclonic separator 8 separation by the catalyzer of gas-solid sharp separation device separates once more, and catalyzer turns back to stripping zone 4 through the dipleg of cyclonic separator 8, and gaseous products gets into collection chamber 10 after outlet line 11 gets into follow-up centrifugal station.Be divided into two portions by gas-solid sharp separation equipment 3 and cyclonic separator 8 isolated reclaimable catalysts through behind the stripping; A part is through turning back to the bottom of reaction zone 2 through catalyst recirculation inclined tube 5 after interchanger 7 heat exchange; A part gets into coke-burning regeneration in the revivifier breeding blanket 18 through inclined tube 6 to be generated in addition; The flue gas that the coke burning generates gets into follow-up energy-recuperation system through cyclonic separator 13 backs through exhanst gas outlet pipeline 21, and a regenerated catalyst part is through in the regenerator sloped tube 12 Returning reactor reaction zones 2.A regenerated catalyst part gets into degas zone 17, after the degassing, gets into riser tube 20, contacts with second raw material, and the product of generation carries catalyzer and gets into reactor drum negative area 8.
Through embodiment the present invention is done further elaboration below, but be not limited only to present embodiment.
Embodiment
[embodiment 1～2]
In reaction-regenerative device as shown in Figure 1, catalyst type is seen table 1.The reactor reaction zone medial temperature is 450 ℃, and the gas phase linear speed is 1.25 meter per seconds, and purity is 99.5% methanol feeding, and the methyl alcohol weight hourly space velocity is 8 hours
-1, the regenerator sloped tube mass flow of catalyst is 1.0: 1 with the ratio of methanol feeding mass rate, and the revivifier medial temperature is 650 ℃, and the spent agent carbon deposition quantity is 4.8% (weight), and the regenerated catalyst carbon deposition quantity is 0.25% (weight).Riser tube is built in the revivifier.Riser tube is one, and second raw material is mixed c 4～carbon six hydrocarbon (wherein carbon four mass content account for 92%) of 90% for the alkene mass content, and adds the water vapour of 10% (weight); With the second raw materials mix charging; The riser tube temperature of reaction is 610 ℃, and the gas phase linear speed is 7 meter per seconds, and regenerated catalyst 20% returns 1/2 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube; 80% entering is built in the riser tube in the revivifier; Keep the stability of catalyst flow control, product stream I and product stream II adopt online gas chromatographic analysis, and experimental result is seen table 1.
Table 1
| Parameter | Catalyst type | Low-carbon alkene carbon back yield, % weight |
| Embodiment 1 | SAPO-18 | 85.47 |
| Embodiment 2 | SAPO-34 | 88.76 |
[embodiment 3～4]
According to embodiment 2 described condition and steps, just change temperature of reactor, experimental result is seen table 2.
Table 2
| Parameter | Temperature of reaction, ℃ | Low-carbon alkene carbon back yield, % |
| Embodiment | ||
| 3 | 400 | 84.08 |
| |
500 | 88.14 |
[embodiment 5～6]
According to embodiment 2 described condition and steps, just change reactor drum gas phase linear speed, experimental result is seen table 3.
Table 3
| Parameter | The gas phase linear speed, meter per second | Low-carbon alkene carbon back yield, % |
| Embodiment | ||
| 5 | 0.8 | 88.27 |
| |
2.0 | 89.08 |
[embodiment 7～8]
According to embodiment 2 described condition and steps, just change the ratio of regenerator sloped tube mass flow of catalyst and methanol feeding mass rate, experimental result is seen table 4.
Table 4
[embodiment 9]
According to embodiment 2 described condition and steps, regenerated catalyst 80% returns fluidized-bed reactor through regenerator sloped tube, and 20% gets into and is built in the riser tube in the revivifier, and low-carbon alkene carbon back yield is 84.76% weight.
[embodiment 10～11]
According to embodiment 2 described condition and steps, just change the riser tube temperature of reaction, experimental result is seen table 5.
Table 5
[embodiment 12～13]
According to embodiment 2 described condition and steps, just change riser tube gas phase linear speed, experimental result is seen table 6.
Table 6
| Parameter | Riser tube gas phase linear speed, meter per second | Low-carbon alkene carbon back yield, % |
| Embodiment | ||
| 12 | 5.0 | 89.11 |
| |
10.0 | 87.10 |
[embodiment 14]
According to embodiment 2 described condition and steps, regenerated catalyst 20% returns 1/3 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube, and low-carbon alkene carbon back yield is 86.76% weight.
[embodiment 15]
According to embodiment 2 described condition and steps, regenerated catalyst 20% returns 1/5 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube, and low-carbon alkene carbon back yield is 84.99% weight.
[embodiment 16]
According to embodiment 2 described condition and steps, regenerated catalyst 20% returns 2/3 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube, and low-carbon alkene carbon back yield is 88.73% weight.
[comparative example 1]
According to embodiment 2 described condition and steps, riser tube just is not set, regenerated catalyst all returns fluidized-bed reactor reaction zone bottom, and low-carbon alkene carbon back yield is 80.28% weight.
[comparative example 2]
According to embodiment 2 described condition and steps, just regenerated catalyst all returns fluidized-bed reactor reaction zone bottom, and low-carbon alkene carbon back yield is 87.25% weight.
Obviously, adopt method of the present invention, can reach the purpose that improves yield of light olefins, have bigger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (10)
1. the method for a preparing low carbon olefin hydrocarbon with methanol said method comprising the steps of:
(a) first raw material that is mainly methyl alcohol contacts with sieve catalyst in fluidized-bed reactor, generates the product stream I that comprises low-carbon alkene, forms carbon deposition catalyst simultaneously;
(b) said carbon deposition catalyst gets into revivifier regeneration through inclined tube to be generated, forms regenerated catalyst;
(c) a said regenerated catalyst part is returned 1/5～2/3 reaction zone height place of fluidized-bed reactor reaction zone through regenerator sloped tube; A part gets into riser tube; Contact with second raw material, generate the product stream II that comprises low-carbon alkene, carry catalyzer and get into said fluidized-bed reactor negative area.
2. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1, it is characterized in that at least a in SAPO-18, SAPO-34 of said molecular screening; Said fluidized-bed reactor is a fast fluidized bed.
3. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 2, it is characterized in that said molecular screening is from SAPO-34.
4. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1, it is characterized in that said regenerated catalyst gets into riser tube after outgasing, riser tube is built in the revivifier, and degas zone is built in the revivifier.
5. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1, it is characterized in that said second raw material is the alkene of carbon four～carbon six.
6. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1, it is characterized in that said riser tube quantity is at least 1.
7. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1, it is characterized in that the shared cover separation process of said product stream I and product stream II.
8. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1; It is characterized in that reaction conditions is in the said fluidized-bed reactor: temperature of reaction is 400～500 ℃; The gas phase linear speed is 0.8～2.0 meter per second, and the regenerator sloped tube mass flow of catalyst is 0.6～2.0: 1 with the ratio of the mass rate of first raw material.
9. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1, it is characterized in that reaction conditions is in the said riser tube: temperature of reaction is 550～650 ℃, and the gas phase linear speed is 5～10 meter per seconds.
10. according to the method for the said preparing low carbon olefin hydrocarbon with methanol of claim 1, it is characterized in that 1/3～2/3 reaction zone height place of fluidized-bed reactor reaction zone is returned through regenerator sloped tube in 20～50% of said regenerated catalyst weight, 50～80% get into riser tubes.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145518A (en) * | 2013-03-18 | 2013-06-12 | 武汉工程大学 | One-step synthesis of ethylene by taking carbon dioxide and water or methanol as raw materials |
| CN112778070A (en) * | 2019-11-09 | 2021-05-11 | 洛阳维达石化工程有限公司 | Method and equipment for pre-hydrocarbon pooling of catalyst |
| 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 |
| CN113387765A (en) * | 2020-03-13 | 2021-09-14 | 中国石油化工股份有限公司 | Method for preparing olefin by using methanol as raw material |
| CN113493367A (en) * | 2020-03-19 | 2021-10-12 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene and fluidized bed reaction-regeneration device |
| CN115304442A (en) * | 2021-05-08 | 2022-11-08 | 国家能源投资集团有限责任公司 | Preparation of C from methanol 2 -C 3 Process and apparatus for olefins |
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| CN101279875A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for increasing production of ethylene and propone |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103145518A (en) * | 2013-03-18 | 2013-06-12 | 武汉工程大学 | One-step synthesis of ethylene by taking carbon dioxide and water or methanol as raw materials |
| CN112778070A (en) * | 2019-11-09 | 2021-05-11 | 洛阳维达石化工程有限公司 | Method and equipment for pre-hydrocarbon pooling of catalyst |
| 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 |
| CN113387765A (en) * | 2020-03-13 | 2021-09-14 | 中国石油化工股份有限公司 | Method for preparing olefin by using methanol as raw material |
| CN113493367A (en) * | 2020-03-19 | 2021-10-12 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene and fluidized bed reaction-regeneration device |
| CN113493367B (en) * | 2020-03-19 | 2024-05-28 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene and fluidized bed reaction-regeneration device |
| CN115304442A (en) * | 2021-05-08 | 2022-11-08 | 国家能源投资集团有限责任公司 | Preparation of C from methanol 2 -C 3 Process and apparatus for olefins |
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| CN102464524B (en) | 2015-04-08 |
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