CN101306969A - Reaction device for preparing low-carbon olefin from oxygen-containing compounds - Google Patents
Reaction device for preparing low-carbon olefin from oxygen-containing compounds Download PDFInfo
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- CN101306969A CN101306969A CNA2007100407022A CN200710040702A CN101306969A CN 101306969 A CN101306969 A CN 101306969A CN A2007100407022 A CNA2007100407022 A CN A2007100407022A CN 200710040702 A CN200710040702 A CN 200710040702A CN 101306969 A CN101306969 A CN 101306969A
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Abstract
The invention relates to a reaction device used to make low-carbon olefin by oxygen compound, mainly solving the problems of the prior art including low device productive capacity, low selectivity of lowcarbon olefin, low circulating load of catalyst and great temperature gradient of reactor. The reaction device solves the problems better through adopting the following technical proposal that: the reaction device mainly comprises a first fluidized bed reactor, a second fluidized bed reactor and a regenerator, wherein the first fluidized bed reactor or the second fluidized bed reactor comprises a feed port 1 or 13, a discharge port 7, a reaction zone 2, a sedimentation section 4, a steam stripping section 3, a cyclone separator 5 and a gas-solid quick separating device 16; the bottom of the steam stripping section 3 of the first fluidized bed reactor is connected with the bottom of the reaction zone of the second fluidized bed reactor through a pipeline 8; the regenerator comprises a regenerating zone 15, a gas-solid quick separating zone 17, a regenerator sedimentation section 18, a regenerator steam stripping section 24 and a regenerator cyclone separator 19; the bottom of the regenerator is provided with a regenerating medium inlet 14; the upper part of the regenerating zone 15 is provided with a gas-solid quick separating device 17; the regenerator sedimentation section 18 is provided inside with a cyclone separator 19, while the top is provided with a smoke outlet 20; the bottom of the steam stripping section 3 of the second fluidized bed reactor is connected with the bottom of the regenerating zone 15 of the regenerator through a pipeline 12; and the bottom of the regenerator steam stripping section 24 is connected with the bottom of the reaction zone 2 of the second fluidized bed reactor through a pipeline 22. Moreover, the reaction device can be used in the industrial production of lowcarbon olefin.
Description
Technical field
The present invention relates to a kind of reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds.
Background technology
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 (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 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 US 4499327 patents 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.
Announced among the US 6166282 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.But the single series processing power of the described fast fluidized bed reactor of this method is lower.
In addition, guarantee high selectivity of light olefin, need long-pending a certain amount of carbon of on the SAPO-34 catalyzer.The method that relates to catalyzer coke content in a kind of MTO of control reactor reaction zone in the US20060025646 patent is the catalyzer part of inactivation to be sent into the breeding blanket make charcoal, and another part decaying catalyst turns back to reaction zone and continues reaction.Because the agent of MTO technology alcohol is than very little, coking yield is lower, if, can make that the catalyst flow between reactor and the revivifier is less in the degree of making charcoal of revivifier inner control catalyzer, and very high to the requirement of catalyst flow control.
Art methods exists all that plant capacity is low, revivifier is made charcoal and is difficult to the problem of aspects such as controlling, the catalyst recirculation amount is less.
Summary of the invention
Technical problem to be solved by this invention is the problem that the plant capacity that exists in the prior art is low, selectivity of light olefin is low, the catalyst recirculation amount is little, the temperature of reactor gradient is big, and a kind of new reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds is provided.This device is used for the production of low-carbon alkene, has the advantage that the high and low carbon olefin selectivity of plant capacity height, catalyst recirculation amount are big, the temperature of reactor gradient is little.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds, reaction unit mainly comprises first class bed bioreactor, second fluidized-bed reactor and revivifier, and the first class bed bioreactor or second fluidized-bed reactor include opening for feed 1 or 13, discharge port 7, reaction zone 2, settling section 4, stripping stage 3, cyclonic separator 5, fast gas-solid separator 16; Opening for feed 1 or 13 is positioned at reactor bottom separately, and discharge port 7 is positioned at each autoreactor top; The bottom of first class bed bioreactor stripping stage 3 links to each other by pipeline 8 with the reaction zone of second fluidized-bed reactor bottom; Revivifier comprises breeding blanket 15, gas-solid sharp separation district 17, revivifier settling section 18, revivifier stripping stage 24, revivifier cyclonic separator 19; Regenerator bottoms has regenerating medium inlet 14, and 15 tops, breeding blanket are provided with fast gas-solid separator 17, and cyclonic separator 19 is arranged in the revivifier settling section 18, and the top has exhanst gas outlet 20; The bottom of the bottom of the second fluidized-bed reactor stripping stage 3 and the breeding blanket of revivifier 15 links to each other by pipeline 12; The bottom of the bottom of revivifier stripping stage 24 and the second fluidized-bed reactor reaction zone 2 links to each other by pipeline 22.
In the technique scheme, described first class bed bioreactor, second fluidized-bed reactor and revivifier are fast fluidized bed; The reaction zone bottom of the bottom of the second fluidized-bed reactor stripping stage and first class bed bioreactor links to each other by pipeline 9; The bottom of the bottom of revivifier stripping stage and first fluidized bed reactor reaction zone links to each other by pipeline 21; The bottom of the bottom of first class bed bioreactor stripping stage and the breeding blanket of revivifier links to each other by pipeline 25; The bottom of first class bed bioreactor stripping stage links to each other by pipeline 10 with the bottom of first fluidized bed reactor reaction zone; The bottom of the bottom of the second fluidized-bed reactor stripping stage and the second fluidized-bed reactor reaction zone links to each other by pipeline 11; Fast gas-solid separator 16 is positioned at the top of fluidized-bed reactor reaction zone separately; Cyclonic separator is positioned at the inside of fluidized-bed reactor settling section 4 separately; The diameter ratio of the diameter of fast gas-solid separator 16 and first class bed bioreactor or the second fluidized-bed reactor reaction zone 2 is 0.1～0.5: 1; Cyclonic separator 5 in the first class bed bioreactor or second fluidized-bed reactor is 1～3 grade, and the cyclonic separator 19 in the revivifier settling section 18 is 1～3 grade.
Because the methanol molecules amount is little, it is quite big to reach the required reactor volume of up to a million tons methyl alcohol treatment scale, adding methanol conversion is may add a certain amount of thinner in the low-carbon alkene reaction process in order to improve the selectivity of low-carbon alkene, to reach certain treatment scale like this, required reactor diameter can be bigger, and the increase of reactor diameter is higher for the requirement meeting of aspects such as gas-solid flow distribution, inner member, back-mixing control.As calculated, realize 1,000,000 tons/year methyl alcohol treatment scale, the diameter of single series reactor will reach more than 10 meters.The reactor that diameter is so big can make gas-solid in the reactor skewness that flows, and the back-mixing degree strengthens, because the MTO reaction is strong exothermal reaction, can make also that therefore the thermograde in the reactor strengthens, and these factors all will have a strong impact on product selectivity.In addition, because the coking yield of methanol to olefins reaction is lower, but also the average coke content that needs to guarantee catalyst in reactor causes the catalyst recirculation amount in the reaction-regeneration system very little on required level, and is very high to the control requirement of catalyst flow.The present invention adopts a kind of fluidized bed reactor system, sets up two fluidized-bed reactors, can realize bigger methyl alcohol treatment scale under the less situation of single series reactor diameter.Exchange owing to catalyzer between two reactors, make that the intrasystem catalyzer coke content adjustment of entire reaction is more flexible, on this basis, can improve the intensity of making charcoal of revivifier, thereby increase " carbon is poor " of reclaimable catalyst and regenerated catalyst, make that the catalyst recirculation quantitative change in the reaction-regeneration system is big, flow control is more prone to.
Adopt technical scheme of the present invention: the reaction zone bottom of the bottom of the second fluidized-bed reactor stripping stage and first class bed bioreactor links to each other by pipeline 9; The bottom of the bottom of revivifier stripping stage and first fluidized bed reactor reaction zone links to each other by pipeline 21; The bottom of the bottom of first class bed bioreactor stripping stage and the breeding blanket of revivifier links to each other by pipeline 25; The bottom of first class bed bioreactor stripping stage links to each other by pipeline 10 with the bottom of first fluidized bed reactor reaction zone; The bottom of the bottom of the second fluidized-bed reactor stripping stage and the second fluidized-bed reactor reaction zone links to each other by pipeline 11; Fast gas-solid separator 16 is positioned at the top of fluidized-bed reactor reaction zone separately; Cyclonic separator is positioned at the inside of fluidized-bed reactor settling section 4 separately; The diameter ratio of the diameter of fast gas-solid separator 16 and first class bed bioreactor or the second fluidized-bed reactor reaction zone 2 is 0.1～0.5: 1; Cyclonic separator 5 in the first class bed bioreactor or second fluidized-bed reactor is 1～3 grade, and the cyclonic separator 19 in the revivifier settling section 18 is 1～3 grade, and yield of light olefins can reach 77.15% (weight), has obtained better technical effect.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
Among Fig. 1,1 is the feeding line of first fluidized bed reactor bottom; 2 is the fluidized-bed reactor reaction zone; 3 is stripping stage; 4 is the settling section of fluidized-bed reactor; 5 is the reactor internal cyclone separators; 6 is collection chamber; 7 is discharge port; 8 is the first class bed bioreactor is carried catalyzer in second fluidized-bed reactor pipeline; 9 is second fluidized-bed reactor is carried catalyzer in the first class bed bioreactor pipeline; 10 is the line of pipes that first class bed bioreactor stripping stage catalyzer returns the reaction zone bottom; 11 is the line of pipes that the catalyzer of the second fluidized-bed reactor stripping stage returns reaction zone 2 bottoms; 12 be in second fluidized-bed reactor behind the stripping reclaimable catalyst enter the line of pipes of revivifier; 13 is the feeding line of second fluidized-bed reactor bottom; 14 is the opening for feed of revivifier; 15 is the revivifier breeding blanket; 16 is the gas-solid sharp separation section of fluidized-bed reactor; 17 is the gas-solid sharp separation section on top, revivifier breeding blanket; 18 is the revivifier settling section; 19 is the revivifier internal cyclone separators; 20 is exhanst gas outlet; 21 return the line of pipes of first fluidized bed reaction zone for regenerated catalyst; 22 return the line of pipes of second fluidized bed reaction zone for regenerated catalyst; 23 is reactive system; 24 is regenerated catalyst stripper; 25 enter the line of pipes of revivifier for reclaimable catalyst behind the stripping in the first class bed bioreactor.
Methyl alcohol enters respectively the reaction zone 2 of first class bed bioreactor and second fluidized bed reactor from feeding line 1 and 13, contact the logistics that generation contains catalyst dust, ethene, propylene with catalyst, after cyclone separator in each autoreactor settling section 45 separates respectively, the gas phase that contains ethene, propylene enters collection chamber 6 from reactor head separately, enter follow-up centrifugal station from outlet 7 discharges at collection chamber 6 tops, isolated catalyst dust sedimentation or return the separately stripping section 3 of fluidized-bed reactor settling section 4 bottoms from the catalyst dipleg of cyclone separator 5 bottoms separately, enter 15 bottoms, regenerator renewing zone through stripping rear portion catalyst by pipeline 12 or 25, part catalyst enters the bottom of another fluidized-bed reactor by pipeline 8,9, and a part of catalyst returns the separately reaction zone 2 of fluidized-bed reactor bottom by pipeline 10,11. Wait the catalyst of regenerating behind regenerator regeneration, stripper 24 strippings, part catalyst returns first fluidized bed reactor lower part reaction zone by pipeline 21, part catalyst returns second fluidized bed reactor lower reaction zone by pipeline 22, and the flue gas of generation is discharged by exhanst gas outlet 20 after separating through the cyclone separator 19 in the regenerator.
The invention will be further elaborated below by embodiment, but be not limited only to present embodiment.
Embodiment
[embodiment 1～4]
In reaction-regenerative device as shown in Figure 1, revivifier adopts fast fluidized bed, and lift gas is an air, 600 ℃ of regeneration temperatures.Two reactors all adopt fast fluidized bed, and the gas superficial velocity in each reactor is 1.2 meter per seconds, and temperature of reaction is 425 ℃, pure methanol feeding, and wherein 40% (weight) enters the first class bed bioreactor, and the methyl alcohol weight space velocity is 3 hours
-1, be 0MPa in gauge pressure reaction and regeneration pressure.First class bed bioreactor stripping stage links to each other with the second fluidized-bed reactor reaction zone by pipeline 8, and the weight ratio of the catalyst flow in catalyst flow and the pipeline 25,10 is 1: 2: 3.The second fluidized-bed reactor stripping stage links to each other with first fluidized bed reactor reaction zone by pipeline 9, and the weight ratio of the catalyst flow in catalyst flow and the pipeline 12,11 is 1: 2: 3.Fast gas-solid separator 16 is positioned at the top of fluidized-bed reactor reaction zone separately, and cyclonic separator is positioned at the inside of fluidized-bed reactor settling section 4 separately; The diameter ratio of the diameter of fast gas-solid separator 16 and first class bed bioreactor or the second fluidized-bed reactor reaction zone 2 is 0.12: 1; Cyclonic separator 5 in the first class bed bioreactor or second fluidized-bed reactor is 1 grade.Cyclonic separator 19 in the revivifier settling section 18 is 1 grade.The thief hole of regenerator and spent agent lays respectively on pipeline 21 and the pipeline 12, and infrared carbon sulphur high speed analysis instrument is adopted in the analysis of carbon content on the catalyzer.The internal circulating load of catalyzer is remained on a rational value, make that system is stable, control is convenient, the catalyst recirculation amount is 2 with the ratio of methyl alcohol combined feed total feed mass rate.Catalyzer adopts the SAPO-34 modified catalyst of spray-dried moulding.The reactor outlet product adopts online gas chromatographic analysis, and experimental result sees Table 1.
Table 1
| Embodiment | Breeding blanket gas phase superfacial velocity, meter per second | The average coke content of reaction zone inner catalyst, % (weight) | The regenerator coke content, % (weight) | Ethene carbon back yield, % (weight) | Propylene carbon back yield, % (weight) | Ethene+propylene carbon back yield, % (weight) |
| |
0.2 | 2.81 | 0.05 | 36.83 | 39.56 | 76.39 |
| Embodiment 2 | 0.5 | 5.26 | 0.41 | 40.46 | 36.67 | 77.13 |
| Embodiment 3 | 1.0 | 5.81 | 0.97 | 42.34 | 32.43 | 74.77 |
| Embodiment 4 | 1.5 | 6.74 | 2.03 | 45.76 | 28.25 | 74.01 |
[embodiment 5]
According to embodiment 2 described conditions, changing the diameter of fast gas-solid separator 16 and the diameter ratio of the first class bed bioreactor or the second fluidized-bed reactor reaction zone 2 is 0.5: 1; Cyclonic separator 5 in the first class bed bioreactor or second fluidized-bed reactor is 3 grades.Cyclonic separator 19 in the revivifier settling section 18 is 3 grades, and experimental result is: ethene carbon back yield is 39.97% (weight), and propylene carbon back yield is 37.18% (weight), and ethene+propylene carbon back yield is 77.15% (weight).
Claims (8)
1, a kind of reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds, reaction unit mainly comprises first class bed bioreactor, second fluidized-bed reactor and revivifier, and the first class bed bioreactor or second fluidized-bed reactor include opening for feed (1) or (13), discharge port (7), reaction zone (2), settling section (4), stripping stage (3), cyclonic separator (5), fast gas-solid separator (16); Opening for feed (1) or (13) are positioned at reactor bottom separately, and discharge port (7) is positioned at each autoreactor top; The bottom of first class bed bioreactor stripping stage (3) links to each other by pipeline (8) with the reaction zone of second fluidized-bed reactor bottom; Revivifier comprises breeding blanket (15), gas-solid sharp separation district (17), revivifier settling section (18), revivifier stripping stage (24), revivifier cyclonic separator (19); Regenerator bottoms has regenerating medium inlet (14), and top, breeding blanket (15) is provided with fast gas-solid separator (17), and cyclonic separator (19) is arranged in the revivifier settling section (18), and the top has exhanst gas outlet (20); The bottom of the breeding blanket (15) of the bottom of the second fluidized-bed reactor stripping stage (3) and revivifier links to each other by pipeline (12); The bottom of the bottom of revivifier stripping stage (24) and the second fluidized-bed reactor reaction zone (2) links to each other by pipeline (22).
2,, it is characterized in that first class bed bioreactor, second fluidized-bed reactor and revivifier are fast fluidized bed according to the described reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds of claim 1.
3,, it is characterized in that the bottom of the second fluidized-bed reactor stripping stage and the reaction zone bottom of first class bed bioreactor link to each other by pipeline (9) according to the described reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds of claim 1.
4,, it is characterized in that the bottom of revivifier stripping stage and the bottom of first fluidized bed reactor reaction zone link to each other by pipeline (21) according to the described reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds of claim 1.
5,, it is characterized in that the bottom of the breeding blanket of the bottom of first class bed bioreactor stripping stage and revivifier links to each other by pipeline (25) according to the described reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds of claim 1.
6,, it is characterized in that the bottom of first class bed bioreactor stripping stage and the bottom of first fluidized bed reactor reaction zone link to each other by pipeline (10) according to the described reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds of claim 1; The bottom of the bottom of the second fluidized-bed reactor stripping stage and the second fluidized-bed reactor reaction zone links to each other by pipeline (11).
7, according to the described reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds of claim 1, it is characterized in that fast gas-solid separator (16) is positioned at the top of fluidized-bed reactor reaction zone separately, cyclonic separator is positioned at the inside of fluidized-bed reactor settling section (4) separately;
8,, it is characterized in that the diameter of fast gas-solid separator (16) and the diameter ratio of the first class bed bioreactor or the second fluidized-bed reactor reaction zone (2) are 0.1～0.5: 1 according to the described reaction unit that is used for preparing low-carbon olefin from oxygen-containing compounds of claim 1; Cyclonic separator (5) in the first class bed bioreactor or second fluidized-bed reactor is 1～3 grade.Cyclonic separator (19) in the revivifier settling section (18) is 1～3 grade.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497016B (en) * | 2009-01-16 | 2011-05-11 | 华中科技大学 | Double-connected fluidized bed reaction device with granules in internal circulation |
| CN102276388A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Reaction device for preparing light olefin from oxygen-containing compound |
| CN102649667A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Method for catalytic dehydration of ethanol |
| CN102649668A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Method for preparing ethylene from ethanol |
| CN101402539B (en) * | 2008-11-21 | 2013-04-10 | 中国石油化工股份有限公司 | Process for producing light olefins with methanol or dimethyl ether |
| CN106794437A (en) * | 2014-10-10 | 2017-05-31 | 埃克森美孚研究工程公司 | The apparatus and method of gasoline, alkene and aromatic compounds are manufactured by oxygenatedchemicals |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6166282A (en) * | 1999-08-20 | 2000-12-26 | Uop Llc | Fast-fluidized bed reactor for MTO process |
| CN100363463C (en) * | 2002-10-18 | 2008-01-23 | 埃克森美孚化学专利公司 | Multiple riser reactor with centralized catalyst return |
-
2007
- 2007-05-16 CN CN2007100407022A patent/CN101306969B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402539B (en) * | 2008-11-21 | 2013-04-10 | 中国石油化工股份有限公司 | Process for producing light olefins with methanol or dimethyl ether |
| CN101497016B (en) * | 2009-01-16 | 2011-05-11 | 华中科技大学 | Double-connected fluidized bed reaction device with granules in internal circulation |
| CN102276388A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Reaction device for preparing light olefin from oxygen-containing compound |
| CN102276388B (en) * | 2010-06-11 | 2014-07-23 | 中国石油化工股份有限公司 | Reaction device for preparing light olefin from oxygen-containing compound |
| CN102649667A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Method for catalytic dehydration of ethanol |
| CN102649668A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Method for preparing ethylene from ethanol |
| CN102649667B (en) * | 2011-02-25 | 2014-07-02 | 中国石油化工股份有限公司 | Method for catalytic dehydration of ethanol |
| CN106794437A (en) * | 2014-10-10 | 2017-05-31 | 埃克森美孚研究工程公司 | The apparatus and method of gasoline, alkene and aromatic compounds are manufactured by oxygenatedchemicals |
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