CN101269344A - Regenerating apparatus for preparing low carbon olefin hydrocarbon with oxygen-containing compounds conversion - Google Patents
Regenerating apparatus for preparing low carbon olefin hydrocarbon with oxygen-containing compounds conversion Download PDFInfo
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- CN101269344A CN101269344A CNA2008100432461A CN200810043246A CN101269344A CN 101269344 A CN101269344 A CN 101269344A CN A2008100432461 A CNA2008100432461 A CN A2008100432461A CN 200810043246 A CN200810043246 A CN 200810043246A CN 101269344 A CN101269344 A CN 101269344A
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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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Abstract
The invention relates to a regenerative device used for making a low-carbon olefin by converting an oxonium compound, and mainly aims at solving the problem that the degree of carbon burning of a regenerator is hard to control and the regenerator is hard to operate in the prior art. As the regenerative device used for making the low-carbon olefin by converting the oxonium compound, the device includes a dilute phase 1 of a regenerator and a dense phase 2 of the regenerator; wherein, the lower side of the dense phase 2 of the regenerator is provided with a catalyst inlet 3 while the lower part of the dense phase 2 of the regenerator is provided with a regeneration media inlet 5, the side of the dense phase 2 of the regenerator is provided with a regeneration media complementary inlet 6; the opening of the upper side of the dense phase 2 of the regenerator is connected with an outside heater 9 while the upper part is connected with the dilute phase 1 of the regenerator; the side lower part of the dilute phase 1 of the regenerator is provided with a catalyst outlet 4 and is internally provided with a cyclone separating device 7 while the upper part of the dilute phase 1 of the regenerator is provided with a gas export 8, wherein, the technical proposal that the regeneration media complementary inlet 6 provides diluents for the recovered gas well solves the problem. The regenerative device used for making the low-carbon olefin by converting the oxonium compound can be used in the industrial production of the low-carbon olefin.
Description
Technical field
The present invention relates to a kind of regenerating unit of preparing low carbon olefin hydrocarbon with oxygen-containing compounds conversion.
Technical background
Low-carbon alkene mainly is ethene and propylene, is two kinds of important basic chemical industry raw materials, and 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 low-carbon alkene 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 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) is subjected to increasing attention.
In addition, this area is confessed, adhere to a certain amount of carbon distribution on the SAPO-34 catalyst, help the selectivity of light olefin that keeps higher, and the agent of MTO technology alcohol ratio is very little, and coking yield is lower, realize catalyst circulation amount bigger, that control easily, just need in the renewing zone, the carbon deposition quantity on the catalyst be controlled at certain level, and then reach the purpose of the average carbon deposition quantity of control reaction zone inner catalyst.Therefore, it is crucial how the average carbon deposition quantity of the catalyst in the reaction zone being controlled at certain level in the MTO technology.
The method that relates to carbon deposition quantity of catalyst in a kind of MTO of control reactor reaction zone in US 20060025646 patents is the catalyst part of inactivation to be sent into the renewing zone burn carbon, and another part decaying catalyst turns back to reaction zone and continues reaction.
Can make in the said method that the carbon difference that enters between two strands of interior catalyst of reactor is very big, mix carbon deposition quantity and inhomogeneous on the rear catalyst, and contain the catalyst of more carbon and contain the catalyst of carbon seldom all unfavorable to the selectivity of low-carbon alkene, there is the problem that the selectivity of product fluctuation is big, the purpose selectivity of product is lower.
Summary of the invention
Technical problem to be solved by this invention is the problem of the bad control of the incomplete charcoal regeneration degree of regenerator inner catalyst that exists in the prior art, and a kind of regenerating unit of new preparing low carbon olefin hydrocarbon with oxygen-containing compounds conversion is provided.This device is used for the production of low-carbon alkene, has more advantage of reasonable of the convenient control of regenerator inner catalyst charcoal regeneration degree, regenerator outlet catalyst average product carbon level.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows, and a kind of regenerating unit of converting oxygen-containing compound to low-carbon olefins mainly comprises: the close phase section 2 of regenerator dilute phase section 1 and regenerator; Close phase section 2 side lower parts of regenerator have catalyst inlet 3, the close phase section of regenerator 2 bottoms have regenerating medium inlet 5, side has regenerating medium and replenishes inlet 6, side top opening connects external warmer 9, top links to each other with regenerator dilute phase section 1, regenerator dilute phase section 1 side lower part has catalyst outlet 4, in establish cyclone separator 7, top has exhanst gas outlet 8.
In the technique scheme, regenerator is a fluid bed, and the regenerator preferred version is a turbulent bed.Close phase section 2 sides of regenerator have regenerating medium and replenish inlet 6, and the close phase section 2 of regenerator is 0.1～0.99: 1 with the diameter ratio preferable range of regenerator dilute phase section; It is 1～10 that the close phase section 2 side regenerating mediums of regenerator replenish inlet 6 quantity preferable range; What the regenerating medium of below replenished the close phase section of the regenerator that enters the mouth bottom is 0.1～1 of the close phase section of whole regenerator height apart from preferred version, and each spacing preferred version that replenishes between the inlet is 0.1～0.9 of the close phase section of a regenerator height.The diameter ratio of close phase section 2 of regenerator and regenerator dilute phase section more preferably scope is 0.4～0.8: 1; The additional inlet of the close phase section 2 side regenerating mediums of regenerator 6 quantity more preferably scope are 1～4; The regenerating medium of below replenish the close phase section of the regenerator that enters the mouth bottom distance more preferably scheme be 0.2～0.8 of the close phase section of whole regenerator height, each replenish between the inlet spacing more preferably scheme be 0.2～0.4 of the close phase section of regenerator height.The regenerating medium that close phase section 2 sides of regenerator are replenished is a kind of or mixes for two or more regenerating mediums that regenerating medium comprises: the flue gas that exhanst gas outlet 8 is gone out, air, oxygen or nitrogen; Nitrogen accounted for 1～99.9% (mol ratio) of mixed regeneration medium when two or more regenerating mediums mixed; Preferred version was 70～99% (mol ratios) that nitrogen accounts for the mixed regeneration medium when two or more regenerating mediums mixed.The regenerating medium of the regenerating medium of the close phase section of regenerator 2 bottoms inlet 5 is a kind of or mixes for two or more regenerating mediums that regenerating medium comprises: flue gas, air, oxygen or nitrogen that exhanst gas outlet (8) is gone out; Nitrogen accounted for 1～99% (mol ratio) of mixed regeneration medium when two or more regenerating mediums mixed; Two or more regenerating medium mixing preferred versions for the time nitrogen account for 70～90% (mol ratios) of mixed regeneration medium.The liquid form of external warmer 9 inner catalysts is free convection, can realize regulating the purpose of regeneration temperature by changing the heat-obtaining load.
Is the reaction of low-carbon alkene for adopting the SAPO-34 molecular sieve catalyst with methyl alcohol or dimethyl ether conversion, contains the raising that certain carbon distribution will help selectivity of light olefin on the catalyst.The average carbon deposition quantity of catalyst reactor should be between 3～6% (mass percents), under this catalyst activity levels, can reach higher selectivity of light olefin, when the carbon deposition quantity of catalyst during in 4.5% (mass percent) left and right sides selectivity of light olefin the highest.Therefore, need be in the burning carbon degree of regenerator inner control catalyst.The approach of controlling the burning carbon degree of catalyst has the concentration of oxygen in the control regenerating medium, recovery time, regeneration temperature etc.The present invention preferably controls the degree of burning carbon from regenerating medium oxygen concentration or recovery time, promptly adopt gas-solid to flow for carrying out the regeneration of catalyst in the turbulent bed, control suitable regeneration temperature and regeneration pressure, replenish flue gas in the close phase section of regenerator, the regenerating medium that oxygen concentrations such as nitrogen are lower is made diluent, to reduce the oxygen concentration in the close phase section of regenerator, thereby the reaction rate of carbon distribution and oxygen on the reduction catalyst, in addition, because the adding of diluent has improved the superficial gas velocity of gas in the close phase section of regenerator, thereby reduced time of contact of carbon distribution and oxygen on the catalyst, promptly reduced the reaction time of carbon distribution and oxygen, in conjunction with the acting in conjunction of two aspects, can realize reducing and burn the carbon amount to control the purpose of carbon deposition quantity on the regenerated catalyst.
Adopt method of the present invention, can be implemented in the regenerator inner control and burn the degree of carbon, make regenerated catalyst keep certain phosphorus content to enter reaction zone, also can make carbon distribution on the catalyst granules after the regeneration form certain carbon deposition quantity by circulation pipe and distribute, thereby reach the purpose of the average carbon deposition quantity of control reaction zone inner catalyst.When the average carbon deposition quantity of the catalyst in the reaction zone is controlled suitable value, can make that selectivity of light olefin reaches maximum.Therefore, method of the present invention can be controlled the scope of regeneration rear catalyst carbon deposition quantity in 3～6% (mass percents) well, and this regenerator is simple and convenient in operation, can realize controlling the purpose of regeneration temperature by the load of regulating external warmer, in addition, also can regulate regeneration temperature, obtain better technical effect by the import and export amount that changes the regenerator catalyst.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
Among Fig. 1,1 is regenerator dilute phase section; 2 is the close phase section of regenerator; 3 is catalyst inlet; 4 is catalyst outlet; 5 are the regenerating medium inlet; 6 are the additional inlet of regenerating medium; 7 is cyclone separator; 8 is exhanst gas outlet; 9 is external warmer.
Reclaimable catalyst flows into from the close phase section 2 side lower part catalyst inlets 3 of regenerator, regenerating medium enters from the regenerating medium entrance 5 of the close phase section of regenerator 2 bottoms, close phase section 2 sides of regenerator enter regenerating medium and mainly play the carrier gas effect, carbon distribution on the catalyst and regenerating medium generation oxidation reaction, catalyst after the regeneration flows out from catalyst outlet 4, gas-solid mixture flows out by the exhanst gas outlet 8 of cyclone separator 7 rear flue gases from regenerator dilute phase section 1 top, catalyst granules is got back to regenerator dilute phase section 1 from cyclone separator 7 diplegs, and the temperature of rare close phase is regulated by external warmer 9 in the regenerator. By control regeneration parameter, such as oxygen concentration, recovery time, regeneration temperature etc. in the regenerating medium, can reach the purpose of control regeneration level.
The invention will be further elaborated below by embodiment, but be not limited only to present embodiment.
The specific embodiment
[embodiment 1～5]
In small-sized circulating fluid bed reaction device, regenerative system flow process form is identical with Fig. 1.The close phase section of regenerator is 0.5 with regenerator dilute phase section diameter ratio, and the close phase section of regenerator side has the additional inlet of regenerating medium that 3 spacings equate, is labeled as regenerating medium successively from top to bottom and replenishes the inlet upper, middle and lower, and close phase section is equally divided into 4 sections.Regeneration temperature is controlled at 660 ℃, is 0MPa in the gauge pressure regeneration pressure, and the inlet amount of catalyst is remained on 10.0 kilograms/hour, guarantees catalyst inventory and controlling level in the regenerator.The regenerating medium inlet adopts air feed, its flow be 5.5 mark cubic meters/hour, regenerating medium replenishes inlet and adopts self exhanst gas outlet institute discharged flue gas, nitrogen gas concn is 80～90% (mol ratios) in its flue gas, catalyst adopts the SAPO-34 catalyst of spray-dried moulding, and be used in fixed fluidized bed oxygen compound and transform a certain amount of carbon on the reaction for preparing light olefins rear catalyst surface area, carbon deposition quantity during the present embodiment catalyst inlet is 6.28% (mass percent), and infrared carbon sulphur high speed analysis instrument is adopted in the analysis of carbon content on the catalyst.Experimental result sees Table 1.
Table 1
| Embodiment | The additional inlet of regenerating medium (on) the mark cubic meter/hour | The additional inlet of regenerating medium (in) the mark cubic meter/hour | The additional inlet of regenerating medium (descending) mark cubic meter/hour | Outlet carbon deposition quantity of catalyst % |
| Embodiment | ||||
| 1 | 1.0 | 0 | 0 | 2.82 |
| |
0 | 1.0 | 0 | 2.85 |
| |
0 | 0 | 1.0 | 2.91 |
| Embodiment 4 | 1.0 | 1.0 | 3.85 | |
| Embodiment 5 | 0 | 0 | 2.0 | 3.82 |
[embodiment 6]
According to the condition of embodiment 3, just will replenish smoke inlet and replenish the regenerating medium inlet that inlet changes close phase pars infrasegmentalis down into by regenerating medium, incorporate air into from bottom feed, experimental result is: the outlet carbon deposition quantity of catalyst is 2.93% (mass percent).
[embodiment 7]
According to the condition of embodiment 5, just change the compensation regeneration medium into nitrogen (＞99% mol ratio) by flue gas, experimental result is: the outlet carbon deposition quantity of catalyst is 3.97% (mass percent).
[embodiment 8]
According to the condition of embodiment 5, just the compensation regeneration medium is changed into flue gas 1.0 mark cubic meters/hour with nitrogen 1.0 mark cubic meter/hour mixed feedings, experimental result is: exporting carbon deposition quantity of catalyst is 3.91% (mass percent).
[comparative example 1]
According to the condition of embodiment 1, just will replenish flue gas and cut off, do not add any diluent, experimental result is: the outlet carbon deposition quantity of catalyst is 0.82% (mass percent).
Obviously, adopt method of the present invention, can realize that the regenerator inner catalyst burns the control of carbon degree, thereby reach the purpose of the average carbon deposition quantity of control reaction zone inner catalyst, finally reach the purpose that improves selectivity of light olefin, have bigger technical advantage, can be used in the industrial production of low-carbon alkene.
Claims (6)
1, a kind of regenerating unit of converting oxygen-containing compound to low-carbon olefins mainly comprises: the close phase section of regenerator dilute phase section (1) and regenerator (2); The close phase section of regenerator (2) side lower part has catalyst inlet (3), the close phase section of regenerator (2) bottom has regenerating medium inlet (5), side has regenerating medium and replenishes inlet (6), side top opening connects external warmer (9), top links to each other with regenerator dilute phase section (1), regenerator dilute phase section (1) side lower part has catalyst outlet (4), in establish cyclone separator (7), top has exhanst gas outlet (8).
2, according to the regenerating unit of the described converting oxygen-containing compound to low-carbon olefins of claim 1, it is characterized in that regenerator is a fluid bed, the close phase section of regenerator (2) side has regenerating medium and replenishes inlet (6), and the close phase section of regenerator (2) is 0.1～0.99: 1 with the diameter ratio of regenerator dilute phase section; It is 1～10 that the close phase section of regenerator (2) side regenerating medium replenishes inlet (6) quantity; To replenish the distance of the close phase section of the regenerator that enters the mouth bottom be 0.1～1 of the close phase section of whole regenerator height to the regenerating medium of below, and each spacing of replenishing between the inlet is 0.1～0.9 of the close phase section of a regenerator height.
3, according to the regenerating unit of the described converting oxygen-containing compound to low-carbon olefins of claim 2, it is characterized in that regenerator is a turbulent bed, the close phase section of regenerator (2) is 0.4～0.8: 1 with the diameter ratio of regenerator dilute phase section; It is 1～4 that the close phase section of regenerator (2) side regenerating medium replenishes inlet (6) quantity; To replenish the distance of the close phase section of the regenerator that enters the mouth bottom be 0.2～0.8 of the close phase section of whole regenerator height to the regenerating medium of below, and each spacing of replenishing between the inlet is 0.2～0.4 of the close phase section of a regenerator height.
4, according to the regenerating unit of the described converting oxygen-containing compound to low-carbon olefins of claim 1, the regenerating medium that it is characterized in that the regenerating medium inlet (5) of the close phase section of regenerator (2) regenerating medium that side replenished or the close phase section of regenerator (2) bottom is a kind of or mixes for two or more regenerating mediums that regenerating medium comprises: flue gas, air, oxygen or nitrogen that exhanst gas outlet (8) is gone out.
5,, account for 1～99.9% of mixed regeneration medium with molar ratio computing nitrogen when it is characterized in that two or more regenerating mediums mix according to the regenerating unit of the described converting oxygen-containing compound to low-carbon olefins of claim 4.
6,, account for 70～99% of mixed regeneration medium with molar ratio computing nitrogen when it is characterized in that two or more regenerating mediums mix according to the regenerating unit of the described converting oxygen-containing compound to low-carbon olefins of claim 5.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811072B (en) * | 2009-02-19 | 2011-12-21 | 中国石油化工股份有限公司 | Regeneration control method in methanol-to-olefins reaction process |
| CN102294205A (en) * | 2010-06-24 | 2011-12-28 | 中国石油化工股份有限公司 | Reactor for producing low carbon olefin by using methanol or dimethyl ether |
| CN102463080A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Reaction device for producing low-carbon olefin by taking methanol as raw material |
| CN103539717A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Reaction device for producing benzpyrole |
| CN107282142A (en) * | 2017-07-05 | 2017-10-24 | 洛阳融惠化工科技有限公司 | A kind of renovation process and equipment that catalyst can be controlled to determine charcoal |
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2008
- 2008-04-11 CN CN2008100432461A patent/CN101269344B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811072B (en) * | 2009-02-19 | 2011-12-21 | 中国石油化工股份有限公司 | Regeneration control method in methanol-to-olefins reaction process |
| CN102294205A (en) * | 2010-06-24 | 2011-12-28 | 中国石油化工股份有限公司 | Reactor for producing low carbon olefin by using methanol or dimethyl ether |
| CN102294205B (en) * | 2010-06-24 | 2013-06-19 | 中国石油化工股份有限公司 | Reactor for producing low carbon olefin by using methanol or dimethyl ether |
| CN102463080A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Reaction device for producing low-carbon olefin by taking methanol as raw material |
| CN103539717A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Reaction device for producing benzpyrole |
| CN103539717B (en) * | 2012-07-12 | 2016-05-18 | 中国石油化工股份有限公司 | Produce the reaction unit of indoles |
| CN107282142A (en) * | 2017-07-05 | 2017-10-24 | 洛阳融惠化工科技有限公司 | A kind of renovation process and equipment that catalyst can be controlled to determine charcoal |
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