CN102274760A - Device for generating catalyst for use in preparation of olefins from methanol - Google Patents
Device for generating catalyst for use in preparation of olefins from methanol Download PDFInfo
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- CN102274760A CN102274760A CN2010101999170A CN201010199917A CN102274760A CN 102274760 A CN102274760 A CN 102274760A CN 2010101999170 A CN2010101999170 A CN 2010101999170A CN 201010199917 A CN201010199917 A CN 201010199917A CN 102274760 A CN102274760 A CN 102274760A
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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
- 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
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Abstract
The invention relates to a device for generating catalyst for use in preparation of olefins from methanol. The catalyst reactivation device mainly solves the problem that a regenerator in the technology of preparing olefins from methanol only can provide a regenerated catalyst with the carbon deposition quantity. The device for generating catalyst for use in preparation of olefins from methanol mainly comprises a first regenerated area 4, a second regenerated area 3, an inclined tube to be regenerated 11, a first regenerated inclined tube 5, a second regenerated inclined tube 7, heating equipment 6, gas-solid separation equipment 8 and a settlement area 9, wherein the upper part of the first regenerated area 4 is connected with the settlement area 9, and the lower part of the first regenerated area 4 is connected with the second regenerated area 3; the gas-solid separation equipment 8 is positioned in the settlement area 9; the inclined tube to be regenerated 11 is connected with the lower part of the first regenerated area 4; the first regenerated inclined tube 5 is connected with the first regenerated area 4; the second regenerated inclined tube 7 is connected with the second regenerated area 3; regenerated medium air inlet pipelines are arranged at bottoms of the first regenerated area 4 and the second regenerated area 3; and a flue gas outlet pipeline 10 is arranged on the top of the settlement area 9. By the technical scheme, the problem is better solved. The catalyst reactivation device can be used for the industrial production of low-carbon olefins.
Description
Technical field
The present invention relates to a kind of catalyst regeneration device that is used for methanol-to-olefins.
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 by 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, the alternative materials that is used for light olefin production that one class is important is an oxygenatedchemicals, for example alcohols (methyl alcohol, ethanol), ethers (dimethyl ether, ethyl methyl ether), ester class (dimethyl carbonate, methyl formate) etc., these oxygenatedchemicals can be transformed by coal, natural gas, living beings equal energy source.Some oxygenatedchemicals can reach fairly large production, as methyl alcohol, can be made by coal or natural gas, and technology is very ripe, can realize up to a million tonnes production scale.Because the popularity in oxygenatedchemicals source is added and is transformed the economy that generates light olefin technology, so by the technology of oxygen-containing compound conversion to produce olefine (OTO), particularly the technology by methanol conversion system alkene (MTO) is subjected to increasing attention.
In the US4499327 patent silicoaluminophosphamolecular molecular sieves catalyst is applied to methanol conversion system olefin process and studies in great detail, think that SAPO-34 is the first-selected catalyst of MTO technology.The SAPO-34 catalyst has very high light olefin selectivity, and activity is also higher, and can make methanol conversion is the degree that was less than in reaction time of light olefin 10 seconds, more even reach in the reaction time range of riser.
Announced among the US6166282 that a kind of oxygenate conversion is the technology and the reactor of low-carbon alkene, 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 afterproduct gas separates fast with catalyst, has effectively prevented the generation of secondary response.Through analog computation, to compare with traditional bubbling fluidization bed bioreactor, this fast fluidized bed reactor internal diameter and the required reserve of catalyst all significantly reduce.Adopt bubbling or turbulent fluidized bed regenerator in this method, one section regeneration only is set, existence can only provide a kind of shortcoming of regenerated catalyst of carbon deposition quantity.
Announced among the CN1723262 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 Disengagement zone of setting, catalyst and product gas are separated.This method regenerator is the bubbling bed, and one section regeneration only is set, and existence can only provide a kind of shortcoming of regenerated catalyst of carbon deposition quantity.
Known in the field, to efficiently utilize the carbon four above hydrocarbon that produce in the methanol-to-olefins process, wherein a kind of scheme utilizes the methanol-to-olefins catalyst that it further is converted into low-carbon alkene exactly, but because the similarities and differences of reaction characteristics, it is different that the required carbon deposition quantity of methanol conversion transforms required carbon deposition quantity with carbon four above hydrocarbon, prior art all only is provided with one section regeneration, and existence can only provide a kind of problem of regenerated catalyst of carbon deposition quantity.The present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the problem that regenerator can only provide a kind of regenerated catalyst of carbon deposition quantity in the methanol-to-olefins technology, and a kind of new catalyst regeneration device that is used for methanol-to-olefins is provided.This device is used for the production of low-carbon alkene, has the advantage that regenerator can provide the regenerated catalyst of two kinds of different carbon deposition quantities.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of catalyst regeneration device that is used for methanol-to-olefins, mainly comprise first renewing zone 4, second renewing zone 3, inclined tube 11 to be generated, first regenerator sloped tube 5, second regenerator sloped tube 7, heat-obtaining equipment 6, gas-solid separation equipment 8, decanting zone 9,4 tops, first renewing zone link to each other with decanting zone 9, the bottom links to each other with second renewing zone 3, gas-solid separation equipment 8 is arranged in decanting zone 9, inclined tube 11 to be generated links to each other with the bottom of first renewing zone 4, first regenerator sloped tube 5 links to each other with first renewing zone 4, second regenerator sloped tube 7 links to each other with second renewing zone 3, first renewing zone 4 and 3 bottoms, second renewing zone are equipped with the regenerating medium admission line, and 9 tops, decanting zone are provided with exhanst gas outlet pipeline 10.
In the technique scheme, described regenerating medium is an air; Described catalyst comprises the SAPO-34 molecular sieve; Carbon deposition quantity of catalyst mass fractions in described first regenerator sloped tube 5 are that carbon deposition quantity of catalyst mass fraction in 0.8～2.0%, second regenerator sloped tube 7 is less than 0.5%; Described gas-solid separation equipment 8 is 1～3 grade of cyclone separator; Described heat-obtaining equipment 6 is external; Described catalyst and regenerating medium are the counter current contacting state; Regeneration temperature is 610～650 ℃ in described first renewing zone 4, and regeneration temperature is 650～685 ℃ in second renewing zone 3.
Carbon deposit quality on the catalyst that coke content computational methods of the present invention are certain mass is divided by described catalyst quality.Carbon deposit measuring method on the catalyst is as follows: will mix the catalyst mix that has carbon deposit that comparatively all has, the accurate carbon-bearing catalyst of weighing certain mass then, be put in the pyrocarbon analyzer and burn, the carbon dioxide quality that generates by infrared analysis burning, thus carbonaceous amount on the catalyst obtained.
The preparation method of silicoaluminophosphamolecular 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 the template agent, and the constitutive material mixed liquor obtains through after the crystallization of certain hour at a certain temperature; Once more, molecular sieve presoma, phosphorus source, silicon source, aluminium source, organic formwork agent, water etc. are mixed the back according to certain ratio and after at least 0.1 hour, finally obtain the SAPO molecular sieve at 110～260 ℃ of following hydrothermal crystallizings.The molecular sieve of preparation is mixed with a certain proportion of binding agent, and through obtaining final SAPO catalyst after the operating procedures such as spray-drying, roasting, the percetage by weight of binding agent in molecular sieve is generally between 10～90%.
Because methanol conversion is in the course of reaction of low-carbon alkene, needs to be with on the catalyst a certain amount of carbon, to improve the selectivity of low-carbon alkene.Prior art all only is provided with one section regeneration, and a kind of regenerated catalyst of carbon deposition quantity can only be provided.And, cause yield of light olefins all lower because methanol conversion transforms the different of required catalyst activity with carbon four above hydrocarbon.In the method for the invention, first renewing zone is set, guarantees that the carbon distribution of regenerated catalyst does not burn totally, the regenerated catalyst that will have a certain amount of carbon distribution then directly returns reaction zone, has significantly improved the yield of low-carbon alkene.And, can further generate ethene, propylene by catalytic pyrolysis for the carbon four above hydrocarbon accessory substances that in methanol-to-olefins reaction process, produce.The required catalyst of the carbon four above hydrocarbon pyrolysis requires to have low carbon deposition quantity.Therefore, in the method for the invention, the catalyst in first renewing zone is imported second renewing zone, to burn the entrained carbon distribution of catalyst completely, recover the initial activity of catalyst, will regenerate then completely that regenerated catalyst is used to transform carbon four above hydrocarbon, with increasing output of ethylene and propylene.Therefore, adopt regenerating unit of the present invention, regenerator provides the regenerated catalyst of two kinds of different carbon deposition quantities, is used for methanol to olefins reaction and carbon four above hydrocarbon producing olefin hydrocarbon by catalytic pyrolysis reactions, has improved the yield of low-carbon alkene in the product.
Adopt technical scheme of the present invention: described regenerating medium is an air; Described catalyst comprises the SAPO-34 molecular sieve; Carbon deposition quantity of catalyst mass fractions in described first regenerator sloped tube 5 are that carbon deposition quantity of catalyst mass fraction in 0.8～2.0%, second regenerator sloped tube 7 is less than 0.5%; Described gas-solid separation equipment 8 is 1～3 grade of cyclone separator; Described heat-obtaining equipment 6 is external; Described catalyst and regenerating medium are the counter current contacting state; Regeneration temperature is 610～650 ℃ in described first renewing zone 4, regeneration temperature is 650～685 ℃ in second renewing zone 3, for methanol to olefins reaction provides the regenerated catalyst of carbon deposition quantity mass fraction between 0.8～2.0%, for the above hydrocarbon producing olefin hydrocarbon by catalytic pyrolysis reaction of carbon four provides the carbon deposition quantity mass fraction less than 0.5% regenerated catalyst, obtained better technical effect simultaneously.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
Among Fig. 1,1 is bottom, second renewing zone regenerating medium suction line; 2 is bottom, first renewing zone regenerating medium suction line; 3 is second renewing zone; 4 is first renewing zone; 5 is first regenerator sloped tube; 6 is the regenerator external warmer; 7 is second regenerator sloped tube; 8 is gas-solid cyclone separator; 9 is the regenerator decanting zone; 10 is the regenerated flue gas outlet line; 11 is inclined tube to be generated.
Reclaimable catalyst enters in first renewing zone 4 with regenerating medium from pipeline 2 through inclined tube 11 to be generated and contacts, coke-burning regeneration, the flue gas that the coke burning generates enters follow-up energy-recuperation system through cyclone separator 8 backs by exhanst gas outlet pipeline 10, and the catalyst that 4 regeneration of first renewing zone are finished returns reaction zone by first regenerator sloped tube 5.Remainder catalyst in first renewing zone 4 enter in second renewing zone 3, contacts with regenerating medium from pipeline 1, and coke-burning regeneration, the catalyst of finishing of regenerating enters other reaction zone through second regenerator sloped tube 7.
The invention will be further elaborated below by embodiment, but be not limited only to present embodiment.
The specific embodiment
[embodiment 1]
On small-sized regenerating unit as shown in Figure 1, adopt the full back-mixing heat collector control of external regeneration temperature, gas-solid cyclone separator adopts 2 grades, the first renewing zone regeneration temperature is 630 ℃, the second renewing zone regeneration temperature is 670 ℃, regenerating medium adopts compressed air, adopt the SAPO-34 molecular sieve catalyst, the bed density of first renewing zone is 385 kilograms per cubic meter, the bed density of second renewing zone is 427 kilograms per cubic meter, inclined tube to be generated links to each other with bottom, first renewing zone, catalyst in first renewing zone enters second renewing zone by the pipeline of bottom, first regenerator sloped tube, second regenerator sloped tube and inclined tube to be generated are equipped with the catalyst sampling equipment, the catalyst sample that takes out adopts infrared carbon sulfur analyzer to measure carbon deposition quantity, analysis result is as follows: the reclaimable catalyst carbon deposition quantity is 4.8% (weight), and the first regenerator sloped tube inner catalyst carbon deposition quantity is 1.5% (weight), and the second regenerator sloped tube inner catalyst carbon deposition quantity is 0.18% (weight).
[embodiment 2]
On small-sized regenerating unit as shown in Figure 1, adopt the full back-mixing heat collector control of external regeneration temperature, gas-solid cyclone separator adopts 3 grades, the first renewing zone regeneration temperature is 650 ℃, the second renewing zone regeneration temperature is 685 ℃, regenerating medium adopts compressed air, adopt the SAPO-34 molecular sieve catalyst, the bed density of first renewing zone is 402 kilograms per cubic meter, the bed density of second renewing zone is 439 kilograms per cubic meter, inclined tube to be generated links to each other with bottom, first renewing zone, catalyst in first renewing zone enters second renewing zone by the pipeline of bottom, first regenerator sloped tube, second regenerator sloped tube and inclined tube to be generated are equipped with the catalyst sampling equipment, the catalyst sample that takes out adopts infrared carbon sulfur analyzer to measure carbon deposition quantity, analysis result is as follows: the reclaimable catalyst carbon deposition quantity is 4.77% (weight), and the first regenerator sloped tube inner catalyst carbon deposition quantity is 0.8% (weight), and the second regenerator sloped tube inner catalyst carbon deposition quantity is 0.07% (weight).
[embodiment 3]
On small-sized regenerating unit as shown in Figure 1, adopt the full back-mixing heat collector control of external regeneration temperature, gas-solid cyclone separator adopts 1 grade, the first renewing zone regeneration temperature is 618 ℃, the second renewing zone regeneration temperature is 650 ℃, regenerating medium adopts compressed air, adopt the SAPO-34 molecular sieve catalyst, the bed density of first renewing zone is 395 kilograms per cubic meter, the bed density of second renewing zone is 454 kilograms per cubic meter, inclined tube to be generated links to each other with bottom, first renewing zone, catalyst in first renewing zone enters second renewing zone by the pipeline of bottom, first regenerator sloped tube, second regenerator sloped tube and inclined tube to be generated are equipped with the catalyst sampling equipment, the catalyst sample that takes out adopts infrared carbon sulfur analyzer to measure carbon deposition quantity, analysis result is as follows: the reclaimable catalyst carbon deposition quantity is 4.85% (weight), and the first regenerator sloped tube inner catalyst carbon deposition quantity is 2.0% (weight), and the second regenerator sloped tube inner catalyst carbon deposition quantity is 0.49% (weight).
Obviously, adopt method of the present invention, can reach the purpose that regenerator provides two kinds of different carbon deposition quantity regenerated catalysts, have bigger technical advantage, can be used in the industrial production of low-carbon alkene.
Claims (8)
1. catalyst regeneration device that is used for methanol-to-olefins, mainly comprise first renewing zone (4), second renewing zone (3), inclined tube to be generated (11), first regenerator sloped tube (5), second regenerator sloped tube (7), heat-obtaining equipment (6), gas-solid separation equipment (8), decanting zone (9), top, first renewing zone (4) links to each other with decanting zone (9), the bottom links to each other with second renewing zone (3), gas-solid separation equipment (8) is arranged in decanting zone (9), inclined tube to be generated (11) links to each other with the bottom of first renewing zone (4), first regenerator sloped tube (5) links to each other with first renewing zone (4), second regenerator sloped tube (7) links to each other with second renewing zone (3), first renewing zone (4) and second renewing zone (3) bottom are equipped with the regenerating medium admission line, and top, decanting zone (9) is provided with exhanst gas outlet pipeline (10).
2. according to the described catalyst regeneration device that is used for methanol-to-olefins of claim 1, it is characterized in that described regenerating medium is an air.
3. according to the described catalyst regeneration device that is used for methanol-to-olefins of claim 2, it is characterized in that described catalyst comprises the SAPO-34 molecular sieve.
4. according to the described catalyst regeneration device that is used for methanol-to-olefins of claim 1, it is characterized in that the carbon deposition quantity of catalyst mass fraction in described first regenerator sloped tube (5) is that the interior carbon deposition quantity of catalyst mass fraction of 0.8～2.0%, second regenerator sloped tube (7) is less than 0.5%.
5. according to the described catalyst regeneration device that is used for methanol-to-olefins of claim 1, it is characterized in that described gas-solid separation equipment (8) is 1～3 grade of cyclone separator.
6. according to the described catalyst regeneration device that is used for methanol-to-olefins of claim 1, it is characterized in that described heat-obtaining equipment (6) is external.
7. according to the described catalyst regeneration device that is used for methanol-to-olefins of claim 1, it is characterized in that described catalyst and regenerating medium are the counter current contacting state.
8. according to the described catalyst regeneration device that is used for methanol-to-olefins of claim 1, it is characterized in that the interior regeneration temperature in described first renewing zone (4) is 610～650 ℃, the interior regeneration temperature in second renewing zone (3) is 650～685 ℃.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360198A (en) * | 2012-03-30 | 2013-10-23 | 中国石油化工股份有限公司 | Combined process for preparing propylene from methyl alcohol with high selectivity |
| CN103588605A (en) * | 2012-08-15 | 2014-02-19 | 神华集团有限责任公司 | Method for producing alkene from methanol |
| CN103772091A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Method for manufacturing low-carbon alkene from methanol |
| CN105561895A (en) * | 2014-10-14 | 2016-05-11 | 中国石油化工股份有限公司 | Methanol-to-olefin device with catalyst mixer and reaction method |
| CN105566023A (en) * | 2014-10-14 | 2016-05-11 | 中国石油化工股份有限公司 | High-efficiency mixing methanol-to-olefin reaction-regenerated device and reaction method using the same |
| CN107540496A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | Methanol or the method for dimethyl ether production aromatic hydrocarbons and low-carbon alkene |
| CN107540498A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | By methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene |
| CN107540492A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | By methanol or the method for dimethyl ether production aromatic hydrocarbons and low-carbon alkene |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360198A (en) * | 2012-03-30 | 2013-10-23 | 中国石油化工股份有限公司 | Combined process for preparing propylene from methyl alcohol with high selectivity |
| CN103360198B (en) * | 2012-03-30 | 2015-08-26 | 中国石油化工股份有限公司 | A kind of combination process of methyl alcohol highly selective preparing propone |
| CN103588605A (en) * | 2012-08-15 | 2014-02-19 | 神华集团有限责任公司 | Method for producing alkene from methanol |
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| CN105561895A (en) * | 2014-10-14 | 2016-05-11 | 中国石油化工股份有限公司 | Methanol-to-olefin device with catalyst mixer and reaction method |
| CN105566023A (en) * | 2014-10-14 | 2016-05-11 | 中国石油化工股份有限公司 | High-efficiency mixing methanol-to-olefin reaction-regenerated device and reaction method using the same |
| CN105566023B (en) * | 2014-10-14 | 2017-11-21 | 中国石油化工股份有限公司 | The methanol to olefins reaction regenerating unit and its reaction method efficiently mixed |
| CN105561895B (en) * | 2014-10-14 | 2018-05-11 | 中国石油化工股份有限公司 | Methanol-to-olefins device and reaction method with catalyst mixer |
| CN107540496A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | Methanol or the method for dimethyl ether production aromatic hydrocarbons and low-carbon alkene |
| CN107540498A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | By methanol or the method for dimethyl ether conversion preparing aromatic hydrocarbon and low-carbon alkene |
| CN107540492A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | By methanol or the method for dimethyl ether production aromatic hydrocarbons and low-carbon alkene |
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