CN101333142B - Starting method of reaction-regenerative device for preparing low carbon olefin form methanol - Google Patents
Starting method of reaction-regenerative device for preparing low carbon olefin form methanol Download PDFInfo
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- CN101333142B CN101333142B CN2008100436142A CN200810043614A CN101333142B CN 101333142 B CN101333142 B CN 101333142B CN 2008100436142 A CN2008100436142 A CN 2008100436142A CN 200810043614 A CN200810043614 A CN 200810043614A CN 101333142 B CN101333142 B CN 101333142B
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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
Abstract
The invention relates to a starting method for a reaction-regeneration device which uses methanol to prepare low-carbon olefin, mainly comprising the following steps: a. using an auxiliary combustion chamber to heat air, and then entering the reaction-regeneration device; heating the dense phase temperature of a regenerator to 400-600 DEG C, and heating the temperature of a reactor reaction zone to 150-350 DEG C; b. switching the catalyst from a catalyst storage tank into the regenerator, and injecting the combustion oil to maintain the temperature of the regenerator; c. switching the catalyst from the regenerator into the reactor, and establishing reaction catalyst circulation between the reactor and the regenerator; d. heating the reactor reaction zone to a temperature not less than 350 DEG C, and putting the raw materials containing the methanol in the reactor to contact with the catalyst so as to generate the products containing low-carbon olefin and also form a carbon deposit on the catalyst; e. stop injecting combustion oil to the regenerator; f. stop using the auxiliary combustion chamber. The method has short starting period and light catalyst damage degree, which can be used for low-carbon olefin industrial production.
Description
Technical field
The present invention relates to a kind of starting method of reaction for preparing light olefins from methanol-regenerating unit.
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 light olefin 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 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) receives increasing attention.
In the US4499327 patent 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 light olefin selectivity, and activity is also higher, and can make methanol conversion is the degree that was less than in reaction times of light olefin 10 seconds, more even reach in the reaction time range of riser tube.
Announced among the US6166282 that a kind of oxygenate 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.
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 disengaging zone of setting, catalyzer and product gas are separated.
Reaction for preparing light olefins from methanol-regeneration alkene has the different of essence with traditional catalytic cracking reaction-regeneration system rapidly, and the driving difficulty is also driven big than catalytic cracking.The present invention provides a kind of starting method of new reaction for preparing light olefins from methanol-regenerating unit.
Summary of the invention
The present invention provides a kind of starting method of new reaction for preparing light olefins from methanol-regenerating unit.This method is used for the production of low-carbon alkene, has the advantage that the driving cycle is short, the catalyst impairment degree is light.
The technical scheme that the present invention adopts is following: a kind of starting method of reaction for preparing light olefins from methanol-regenerating unit; Mainly may further comprise the steps: (a) adopt auxiliary chamber to add that warm air is laggard goes into said reaction-regenerative device; The close phase section of revivifier temperature is heated to 400～600 ℃, the reactor reaction zone temperature is heated to 150～350 ℃; (b) from the catalyzer storage tank, change catalyzer over to revivifier, and spray into combustion oil maintenance regenerator temperature; (c) change the catalyzer in the revivifier over to reactor drum, set up the catalyst recirculation between reactor drum and revivifier; (d) with the reactor reaction zone temperature be heated to be not less than 350 ℃ after, feed the raw material that comprises methyl alcohol in the reactor drum, contact with catalyzer, generation comprises the product of low-carbon alkene and on catalyzer, forms carbon deposit; (e) stop to spray into combustion oil to revivifier; (f) inactive auxiliary chamber.
In the technique scheme, the indoor combustion medium of said aid burning is selected from diesel oil, fuel gas; Said catalyzer comprises silicoaluminophosphamolecular molecular sieve; Said combustion oil is a diesel oil; After catalyzer coke content in reactor is greater than 1% weight, stop to spray into combustion oil to revivifier; Catalyzer in the revivifier is changed in the process of reactor drum, continue from the catalyzer storage tank, in revivifier, to change over to catalyzer; Before reactor drum changes catalyzer over to, feed water vapour from revivifier in the reactor drum.
Fuel gas according to the invention mainly contains components such as methane, hydrogen, ethene, propylene.
Because the coking yield of reaction for preparing light olefins from methanol is lower; And the methanol molecules amount is less; Therefore its reaction-regeneration system has the characteristics of " big reactor drum, little revivifier "; Be essentially different with the characteristics of traditional catalytic cracking " little reactor drum, big revivifier ", this makes that also the driving of reaction for preparing light olefins from methanol-regeneration system rapidly is different with traditional circulating fluidized bed starting method, and difficulty is bigger.The present invention adds the catalyzer limit to the method that reactor drum changes catalyzer through adopting the limit to revivifier, has shortened the driving cycle, has reduced the infringement of catalyzer in startup procedure.The heat of revivifier is through spraying into combustion oil and the thermal regeneration air guarantees; After system gets into methanol feedstock; Can accumulate a certain amount of carbon deposit gradually on the catalyzer, when carbon deposit run up to a certain amount of after, the heat of revivifier just can be kept through the burning heat release of carbon deposit; At this moment can remove combustion oil and auxiliary chamber, make reaction-regeneration system smooth running under the thermal equilibrium of self.
Adopt technical scheme of the present invention: the indoor combustion medium of said aid burning is selected from diesel oil, fuel gas; Said catalyzer comprises silicoaluminophosphamolecular molecular sieve; Said combustion oil is a diesel oil; After catalyzer coke content in reactor is greater than 1% weight, stop to spray into combustion oil to revivifier; Catalyzer in the revivifier is changed in the process of reactor drum, continue from the catalyzer storage tank, in revivifier, to change over to catalyzer; Before reactor drum changes catalyzer over to, feed water vapour from revivifier in the reactor drum, the driving cycle, between 2～4 hours, in continuous 50 days operational process, yield of light olefins on average reached 80.5% weight, has obtained better technical effect basically.
Description of drawings
Fig. 1 is the schematic flow sheet of scheme according to the invention.
Among Fig. 1,1 is the reactor feedstocks charging; 2 is reactor reaction zone; 3 are gas-solid sharp separation district; 4 is stripping zone; 5 is reactor drum outer circulation inclined tube; 6 is inclined tube to be generated; 7 is the close phase section of revivifier; 8 is the reactor drum gas-solid cyclone separator; 9 is the reactor drum disengaging zone; 10 are regenerator sloped tube catalyst flow control guiding valve; 11 is the product gas outlet pipeline; 12 is revivifier dilute phase section; 13 is the regenerating medium source line; 14 is inclined tube catalyst flow control guiding valve to be generated; 15 is the revivifier external warmer; 16 is the revivifier gas-solid cyclone separator; 17 is the regenerated flue gas outlet line; 18 is the reactor drum external warmer; 19 is regenerator sloped tube; 20 are steam entering reactor line; 21 is revivifier; 22 is reactor drum; 23 is the combustion oil source line; 24 are the large-scale agent line that adds of regenerator bottoms.
The logistics that comprises methanol feedstock gets in the reaction zone 2 of reactor drum 22 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 disengaging zone 9 through gas-solid sharp separation district 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 follow-up centrifugal station through outlet line 11.Be divided into two portions with cyclonic separator 8 isolated reclaimable catalysts through behind the stripping by gas-solid sharp separation district 3, a part turns back to the bottom of reaction zone 2 through catalyzer outer circulation inclined tube 5; A part is through coke-burning regeneration in the close phase section 7 of inclined tube 6 entering revivifiers 21 to be generated in addition; The flue gas that the coke burning generates gets into follow-up energy-recuperation system through cyclonic separator 16 backs through exhanst gas outlet pipeline 17, and the catalyzer that regeneration is accomplished returns reaction zone 2 through regenerator sloped tube 19.During driving, catalyzer adds in the reaction-regeneration system through the large-scale agent line that adds of regenerator bottoms, and combustion oil gets in the close phase section 7 of revivifier from pipeline 23; Before raw material incision reactor drum, adopt MP steam fluidized catalyst from pipeline 20 incision reactor drums.
Through embodiment the present invention is done further elaboration below, but be not limited only to present embodiment.
Embodiment
[embodiment 1]
Reaction for preparing light olefins from methanol-regeneration system rapidly as shown in Figure 1, reactor drum are fast bed, and revivifier is the bubbling bed; Catalyzer is the SAPO-34 molecular sieve, and the methanol feeding amount is 4.2 tons/hour, and the indoor feeding fuel gas igniting of aid burning is used for regeneration air is heated; Regeneration air is heated the back and gets into revivifier, and revivifier is heated to about 450 ℃, improves regeneration pressure; Make regeneration air to get into reactor drum, and reactor drum is heated to about 230 ℃ through regenerator sloped tube and inclined tube to be generated.Catalyzer is changed over to the revivifier from the catalyzer storage tank through the large-scale agent line that adds; When the regenerator bed material level arrives more than the combustion oil nozzle location 1 meter; And the close phase section of revivifier temperature sprays into combustion oil greater than after 370 ℃ to the close phase section of revivifier, and combustion oil adopts hydrogenated diesel oil.Fast the close phase section of revivifier temperature is risen to more than 550 ℃ after diesel oil sprays into, accelerate in revivifier, to change over to the speed of catalyzer simultaneously; When the revivifier material level reaches 62%, beds did not have cyclone dip-leg, when the close phase section of revivifier temperature is 530 ℃; Open the regenerator sloped tube guiding valve; Change catalyzer over to reactor drum, the catalyzer that changes reactor drum over to gets into disengaging zone and stripping zone through the fast bed reaction zone, and the material level of treating stripping zone has and shows and after temperature obviously rises; Open inclined tube guiding valve to be generated, set up the catalyst recirculation between reactor drum and revivifier gradually; Change over to from revivifier the process of reactor drum at catalyzer, continue to change catalyzer from the catalyzer storage tank over to revivifier, the catalyst inventory in reactor drum and revivifier arrives value; After two devices are set up circulation, when the high temperature catalyst of coming through regenerator sloped tube from revivifier is heated to 380 ℃ of left and right sides with the reactor reaction zone temperature, feed the raw material that comprises methyl alcohol in the reactor drum, reduce quantity of steam according to certain ratio simultaneously.Raw material contacts with the catalyzer of reaction zone, generates to comprise the product of low-carbon alkene and on catalyzer, form carbon deposit; When the reclaimable catalyst carbon deposit reaches 1.5% weight, stop to spray into combustion oil to revivifier; When the reclaimable catalyst carbon deposit reaches 3.3% weight when above, the auxiliary chamber of stopping using.
Whole startup procedure lasts about 3 hours, and in continuous 50 days operational process, yield of light olefins on average reaches 80.5% weight.
Obviously, adopt method of the present invention, can reach and shorten the driving cycle, reduce the purpose of catalyst impairment degree, have bigger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (7)
1. the starting method of methyl alcohol system ethene and propylene reaction-regenerative device may further comprise the steps:
(a) adopt auxiliary chamber to add that warm air is laggard goes into said reaction-regenerative device, the close phase section of revivifier temperature is heated to 400～600 ℃, the reactor reaction zone temperature is heated to 150～350 ℃;
(b) from the catalyzer storage tank, change catalyzer over to revivifier, and spray into combustion oil maintenance regenerator temperature;
(c) change the catalyzer in the revivifier over to reactor drum, set up the catalyst recirculation between reactor drum and revivifier;
(d) with the reactor reaction zone temperature be heated to be not less than 350 ℃ after, feed the raw material that is selected from methyl alcohol in the reactor drum, contact with catalyzer, generation is selected from the product of ethene and propylene and on catalyzer, forms carbon deposit;
(e) stop to spray into combustion oil to revivifier;
(f) inactive auxiliary chamber.
2. according to the starting method of said methyl alcohol system ethene of claim 1 and propylene reaction-regenerative device, it is characterized in that the indoor combustion medium of said aid burning is selected from diesel oil, fuel gas.
3. according to the starting method of said methyl alcohol system ethene of claim 1 and propylene reaction-regenerative device, it is characterized in that said catalyzer is selected from silicoaluminophosphamolecular molecular sieve.
4. according to the starting method of said methyl alcohol system ethene of claim 1 and propylene reaction-regenerative device, it is characterized in that said combustion oil is a diesel oil.
5. according to the starting method of said methyl alcohol system ethene of claim 1 and propylene reaction-regenerative device, it is characterized in that after catalyzer coke content in reactor is greater than 1% weight, stopping to spray into combustion oil to revivifier.
6. according to the starting method of said methyl alcohol system ethene of claim 1 and propylene reaction-regenerative device, it is characterized in that the catalyzer in the revivifier is changed in the process of reactor drum, continue from the catalyzer storage tank, in revivifier, to change over to catalyzer.
7. according to the starting method of said methyl alcohol system ethene of claim 1 and propylene reaction-regenerative device, it is characterized in that from revivifier before reactor drum changes catalyzer over to, feed water vapour in the reactor drum.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100436142A CN101333142B (en) | 2008-07-08 | 2008-07-08 | Starting method of reaction-regenerative device for preparing low carbon olefin form methanol |
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| CN2008100436142A CN101333142B (en) | 2008-07-08 | 2008-07-08 | Starting method of reaction-regenerative device for preparing low carbon olefin form methanol |
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| CN101333142B true CN101333142B (en) | 2012-05-30 |
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| CN102020523B (en) * | 2009-09-10 | 2013-06-05 | 中国石油化工股份有限公司 | Operating method for olefin conversion device |
| CN102276392B (en) * | 2010-06-11 | 2013-12-25 | 中国石油化工股份有限公司 | Starting method of reaction device for preparing low-carbon olefin by use of methanol |
| CN102295503B (en) * | 2010-06-24 | 2014-05-28 | 中国石油化工股份有限公司 | Reaction-regeneration device for preparing low-carbon olefin from methanol |
| CN102463072B (en) * | 2010-11-17 | 2014-07-23 | 中国石油化工股份有限公司 | Reaction device for producing p-xylene |
| CN102875294B (en) * | 2011-07-12 | 2015-01-07 | 中国石油化工股份有限公司 | Start-up method of reaction-regeneration device for preparing low-carbon olefins from methanol |
| CN103121889A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Warm-taking method for preparing low-carbon olefin through conversion of oxygenated chemicals |
| CN102367217B (en) * | 2011-11-25 | 2013-12-18 | 神华集团有限责任公司 | Methanol-to-olefin device and its initiation method |
| CN103193574B (en) * | 2012-01-10 | 2015-01-07 | 中国石油化工股份有限公司 | On-stream method of methanol to light olefin reaction-regeneration device |
| CN103664443B (en) * | 2012-09-05 | 2015-12-16 | 中国石油化工股份有限公司 | The method of replacing of catalyzer in preparing low carbon olefin hydrocarbon by methanol |
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| CN103666534B (en) * | 2012-09-20 | 2015-07-29 | 中国石油化工股份有限公司 | A kind of catalytic cracking unit start-up method |
| CN103666528B (en) * | 2012-09-20 | 2015-07-29 | 中国石油化工股份有限公司 | A kind of catalytic cracking unit start-up method |
| CN103666527B (en) * | 2012-09-20 | 2015-07-29 | 中国石油化工股份有限公司 | A kind of catalytic cracking unit start-up method |
| CN103666532B (en) * | 2012-09-20 | 2015-07-29 | 中国石油化工股份有限公司 | A kind of method that catalytic cracking unit adopts live catalyst to go into operation |
| CN103666533B (en) * | 2012-09-20 | 2015-08-26 | 中国石油化工股份有限公司 | A kind of method that catalytic cracking unit adopts live catalyst to go into operation |
| CN103666529B (en) * | 2012-09-20 | 2015-08-26 | 中国石油化工股份有限公司 | A kind of method that catalytic cracking unit adopts live catalyst to go into operation |
| CN103666526B (en) * | 2012-09-20 | 2015-08-26 | 中国石油化工股份有限公司 | A kind of catalytic cracking unit start-up method |
| CN103666530B (en) * | 2012-09-20 | 2015-08-26 | 中国石油化工股份有限公司 | A kind of catalytic cracking unit start-up method |
| CN103666531B (en) * | 2012-09-20 | 2015-07-29 | 中国石油化工股份有限公司 | A kind of catalytic cracking unit start-up method |
| CN103739419B (en) * | 2012-10-17 | 2015-09-09 | 中国石油化工股份有限公司 | The method of preparing light olefins from methanol |
| CN103772092B (en) * | 2012-10-25 | 2016-04-13 | 中国石油化工股份有限公司 | Methanol conversion is the reaction unit of low-carbon alkene |
| CN105983379B (en) * | 2015-01-28 | 2019-01-25 | 中国石化工程建设有限公司 | A kind of start-up method of organic oxide catalytic cracking aromatic device |
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| US4499327A (en) * | 1982-10-04 | 1985-02-12 | Union Carbide Corporation | Production of light olefins |
| CN101165018A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene |
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2008
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| US4499327A (en) * | 1982-10-04 | 1985-02-12 | Union Carbide Corporation | Production of light olefins |
| CN101165018A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene |
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