CN101941874A - Method for producing low-carbon olefins - Google Patents
Method for producing low-carbon olefins Download PDFInfo
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- CN101941874A CN101941874A CN2009100575474A CN200910057547A CN101941874A CN 101941874 A CN101941874 A CN 101941874A CN 2009100575474 A CN2009100575474 A CN 2009100575474A CN 200910057547 A CN200910057547 A CN 200910057547A CN 101941874 A CN101941874 A CN 101941874A
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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
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Abstract
The invention relates to a method for producing low-carbon olefins and mainly solves the problems of heavy catalyst pollution and low low-carbon olefin yield of the prior art. The method for producing low-carbon olefins comprises the following steps: (a) heating a regeneration area to a first temperature of at least 400 DEG C, and introducing at least part of a catalyst to the regeneration area to contact the part of the catalyst with a regeneration medium; (b) heating the regeneration area to a second temperature of at least 250 DEG C; (c) transferring the catalyst in a regenerator to a reactor, and establishing catalyst circulation between the reactor and the regenerator; (d) introducing a fuel of which the autoignition temperature is between 250 and 400 DEG C and of which the metal impurity content is no more than 10 mg/g into the regeneration area to combust the fuel to heat the catalyst; (e) circulating the heated catalyst to a low-carbon olefin producing reaction area; and (f) under a condition of converting raw materials into low-carbon olefins effectively, contacting the heated catalyst with the raw materials in the reaction area. The method can be used in the industrial production of low-carbon olefins.
Description
Technical field
The present invention relates to a kind of production method of low-carbon alkene.
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 (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 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) is subjected to increasing attention.
In the US4499327 patent silicoaluminophosphamolecular molecular sieves catalyzer is applied to methanol conversion system olefin process and studies in great detail, 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 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 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.
Announced a kind of method of low carbon olefin preparation by using oxygenated chemical among the ZL03811504.2, in the device start-up course, sprayed into heating fuel, be used for heatable catalyst and start reactive system.Wherein, define in this patent and spray into the sulphur that contains in the described fuel and the index of nitrogen, prevent the pollution of catalyzer and the generation of gaseous impurities.
But, for the catalyzer that is used for methanol conversion system alkene, it is far from being enough only being limited to the sulphur, the nitrogen index that contain in the fuel that sprays in the process that starts reactive system, the easiest what catalyzer was polluted is the trace metal that contains in the fuel, may cause irreversible permanent inactivation to catalyzer.Though therefore in the process that starts the methanol to olefins reaction system, can use for reference the startup method of catalytic cracking (FCC) reactive system, but the heating fuel that can be used in the startup of FCC system often can not be used for the methanol-to-olefins system, has the serious problems of catalyst contamination.Therefore, need a kind of method of preparing light olefins from methanol, can guarantee in the process that reactive system starts, to reduce the pollution of catalyzer as far as possible, and can be low-carbon alkene effectively methanol conversion.The present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the problem that the catalyst contamination that exists in the prior art is big, yield of light olefins is low, and a kind of production method of new low-carbon alkene is provided.This method is used for the production of low-carbon alkene, has the advantage that catalyst contamination is little, yield of light olefins is high.
The technical solution used in the present invention is as follows: a kind of production method of low-carbon alkene may further comprise the steps: (a) breeding blanket is heated at least 400 ℃ first temperature, at least a portion catalyzer enters the breeding blanket and contacts with regenerating medium; (b) breeding blanket is heated at least 250 ℃ second temperature; (c) change the catalyzer in the revivifier over to reactor, set up the catalyst recirculation between reactor and revivifier; (d) with spontaneous ignition temperature between 250～400 ℃ and the metals content impurity fuel that is not more than 10 mg/kg enter the breeding blanket burning, heat described catalyzer; (e) the described catalyst recirculation after will heating to the reaction zone of producing low-carbon alkene and; (f) be under the condition of low-carbon alkene effectively, allowing the described catalyzer after heating contact at reaction zone with raw material with feedstock conversion.
In the technique scheme, described raw material comprises methyl alcohol; Described catalyzer comprises SAPO-34; Described fuel is diesel oil; Metallic impurity are selected from least a in basic metal, alkaline-earth metal, nickel or the vanadium; Described condition for validity comprises that temperature of reaction is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the methyl alcohol weight space velocity is 1.0～15.0 hours
-1
In the start-up course of methanol to olefins reaction system, need behind reaction zone, reaction zone can be joined feed temperature to the catalyst recirculation after the revivifier additional heat is with heatable catalyst and assurance heating.Because it is less demanding in the FCC system to the impurity that adds fuel, and methanol to olefins reaction system and catalyzer all have special requirement to heating fuel, in case the pollution of catalyzer generation, so traditional FCC heating raw can not be applicable to the methanol-to-olefins system.What easily activity of such catalysts is caused permanent damage mainly is some metal, as basic metal, alkaline-earth metal, nickel, vanadium etc.Therefore in the start-up course of methanol to olefins reaction system, the foreign matter content in the strict control heating fuel, prevent the irreversible inactivation of catalyzer.Adopt method of the present invention, can address this problem.
Adopt technical scheme of the present invention: described raw material comprises methyl alcohol; Described catalyzer comprises SAPO-34; Described fuel is diesel oil; Metallic impurity are selected from least a in basic metal, alkaline-earth metal, nickel or the vanadium; Described condition for validity comprises that temperature of reaction is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the methyl alcohol weight space velocity is 1.0～15.0 hours
-1, yield of light olefins is up to more than 81.2% weight, has obtained better technical effect.
Description of drawings
Fig. 1 is the schematic flow sheet of scheme of the present 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 outer circulation inclined tube; 6 is inclined tube to be generated; 7 is the close phase section of revivifier; 8 is the reactor gas-solid cyclone separator; 9 is the reactor 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 external warmer; 19 is regenerator sloped tube; 20 enter reactor line for steam; 21 is revivifier; 22 is reactor; 23 is the heating fuel source line; 24 are the large-scale agent line that adds of regenerator bottoms.
The logistics that comprises the methyl alcohol raw material enters in the reaction zone 2 of reactor 22 through feeding line 1, contact with molecular sieve catalyst, reaction generates the product that contains low carbon olefin, carry catalyst to be generated and enter reactor Disengagement zone 9 through the quick Disengagement zone 3 of gas-solid, wherein, most of catalyst that the quick separation equipment 3 of gas-solid is separated enters stripping zone 4, and gas phase product and part are not separated through entering cyclone separator 8 separation again by the catalyst that the quick separation equipment of gas-solid separates, catalyst turns back to stripping zone 4 through the dipleg of cyclone separator 8, and the gas phase product enters follow-up centrifugal station through outlet line 11. Be divided into two parts by the quick Disengagement zone 3 of gas-solid and cyclone separator 8 isolated catalyst to be generated through behind the stripping, a part turns back to the bottom of reaction zone 2 by catalyst outer circulation inclined tube 5; A part enters coke-burning regeneration in the close phase section 7 of regenerator 21 through inclined tube 6 to be generated in addition, enter follow-up energy recovery system by exhanst gas outlet pipeline 17 behind the flue gas process cyclone separator 16 that the coke burning generates, the catalyst that regeneration is finished returns reaction zone 2 by regenerator sloped tube 19. During driving, catalyst adds in the reaction-regeneration system by the large-scale agent line that adds of regenerator bottom, and heating fuel enters in the close phase section 7 of regenerator from pipeline 23; Before raw material incision reactor, adopt the middle pressure steam fluidized catalyst from pipeline 20 incision reactors.
The invention will be further elaborated below by embodiment, 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 is a fast bed, revivifier is a dense bed, and catalyzer is the SAPO-34 molecular sieve, and the methanol feeding amount is 4.2 tons/hour, the indoor feeding fuel gas igniting of aid burning is used for regeneration air is heated, enter revivifier after regeneration air is heated, revivifier is heated to about 400 ℃, improve regeneration pressure, make regeneration air to enter reactor, and reactor is heated to about 230 ℃ by regenerator sloped tube and inclined tube to be generated.Catalyzer is changed over to the revivifier from the catalyzer storage tank by the large-scale agent line that adds, when the regenerator bed material level arrives more than the heating fuel nozzle location 1 meter, and the breeding blanket temperature sprays into hydrogenated diesel oil greater than after 350 ℃ to the close phase section of revivifier, and the metals content impurity in the described hydrogenated diesel oil sees Table 1.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, the catalyzer that changes reactor over to enters disengaging zone and stripping zone through the fast bed reaction zone, and the material level for the treatment of 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 and revivifier gradually; Change over to from revivifier the process of reactor at catalyzer, continue to change catalyzer from the catalyzer storage tank over to revivifier, the catalyst inventory in reactor and revivifier arrives design load; After two devices are set up circulation, when the high temperature catalyst of coming by 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, 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 form carbon deposit on catalyzer; When the reclaimable catalyst carbon deposit reaches 1.5% weight, stop to spray into heating fuel to revivifier; When the reclaimable catalyst carbon deposit reaches 3.3% weight when above, the auxiliary chamber of stopping using.Temperature of reaction in the reactor reaches about 460 ℃, and reaction pressure is counted 0.15MPa with gauge pressure, and the methyl alcohol weight space velocity is 10 hours
-1Whole startup procedure lasts about 3 hours, and in continuous 50 days operational process, yield of light olefins on average reaches 80.5% weight.
[embodiment 2]
According to embodiment 1 described condition, after reactive system started successfully, the temperature of reaction in the reactor changed into about 400 ℃, and the methyl alcohol weight space velocity changes 1.0 hours into
-1, yield of light olefins is 78.7% weight.
[embodiment 3]
According to embodiment 1 described condition, after reactive system started successfully, the temperature of reaction in the reactor changed into about 500 ℃, and the methyl alcohol weight space velocity changes 15.0 hours into
-1, yield of light olefins is 79.5% weight.
[embodiment 4]
According to embodiment 1 described condition, after reactive system started successfully, the reaction pressure in the reactor changed 0.01MPa in gauge pressure, and yield of light olefins is 81.2% weight.
[embodiment 5]
According to embodiment 1 described condition, after reactive system started successfully, the reaction pressure in the reactor changed 0.3MPa in gauge pressure, and yield of light olefins is 77.6% weight.
[comparative example 1]
Be on 1 kilogram/hour the small-sized circulating fluidized bed reaction regeneration device, to have carried out of the influence test of the dissimilar heating fuel of different metal foreign matter content in the laboratory inlet amount, the results are shown in Table 1 catalyzer.
Table 1
| Oil product | Hydrogenated diesel oil | Ordinary diesel oil |
| Basic metal, mg/kg | ＜3 | 6.2 |
| Alkaline-earth metal, mg/kg | ＜4 | 5.7 |
| Nickel, mg/kg | ＜0.1 | 1.2 |
| Vanadium, mg/kg | ＜0.1 | 0.24 |
| With catalyzer duration of contact, |
3 | 3 |
| Oil mass/catalyst weight, kg/kg | 0.05 | 0.05 |
| Yield of light olefins | 80.8 | 79.6 |
Obviously, adopt method of the present invention, can reach the purpose that reduces the catalyst impairment degree, have bigger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (6)
1. the production method of a low-carbon alkene may further comprise the steps:
(a) breeding blanket is heated at least 400 ℃ first temperature, at least a portion catalyzer enters the breeding blanket and contacts with regenerating medium;
(b) breeding blanket is heated at least 250 ℃ second temperature;
(c) change the catalyzer in the revivifier over to reactor, set up the catalyst recirculation between reactor and revivifier;
(d) with spontaneous ignition temperature between 250～400 ℃ and the metals content impurity fuel that is not more than 10 mg/kg enter the breeding blanket burning, heat described catalyzer;
(e) the described catalyst recirculation after will heating to the reaction zone of producing low-carbon alkene and;
(f) be under the condition for validity of low-carbon alkene with feedstock conversion, allowing the described catalyzer after heating contact at reaction zone with raw material.
2. according to the production method of the described low-carbon alkene of claim 1, it is characterized in that described raw material comprises methyl alcohol.
3. according to the production method of the described low-carbon alkene of claim 1, it is characterized in that described catalyzer comprises the SAPO-34 molecular sieve.
4. according to the production method of the described low-carbon alkene of claim 4, it is characterized in that described fuel is diesel oil.
5. according to the production method of the described low-carbon alkene of claim 1, it is characterized in that described metallic impurity are selected from least a in basic metal, alkaline-earth metal, nickel or the vanadium.
6. according to the production method of the described low-carbon alkene of claim 1, it is characterized in that described condition for validity comprises that temperature of reaction is 400～500 ℃, reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the methyl alcohol weight space velocity is 1.0～15.0 hours
-1
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872761A (en) * | 2011-07-12 | 2013-01-16 | 中国石油化工股份有限公司 | Production device of low-carbon olefins |
| CN103772104A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Reaction device for preparing light olefin by methanol |
| CN104372995A (en) * | 2014-10-09 | 2015-02-25 | 赵崇谊 | Intelligent drum brake type anti-theft lock for electric vehicle |
| CN114341317A (en) * | 2019-08-05 | 2022-04-12 | 沙特基础工业全球技术公司 | Additional heat source for naphtha catalytic cracking |
-
2009
- 2009-07-06 CN CN2009100575474A patent/CN101941874A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872761A (en) * | 2011-07-12 | 2013-01-16 | 中国石油化工股份有限公司 | Production device of low-carbon olefins |
| CN103772104A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Reaction device for preparing light olefin by methanol |
| CN103772104B (en) * | 2012-10-25 | 2015-11-18 | 中国石油化工股份有限公司 | The reaction unit of preparing light olefins from methanol |
| CN104372995A (en) * | 2014-10-09 | 2015-02-25 | 赵崇谊 | Intelligent drum brake type anti-theft lock for electric vehicle |
| CN114341317A (en) * | 2019-08-05 | 2022-04-12 | 沙特基础工业全球技术公司 | Additional heat source for naphtha catalytic cracking |
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