CN101333141A - Reaction device for conversing methanol or dimethyl ether to be low carbon olefin - Google Patents
Reaction device for conversing methanol or dimethyl ether to be low carbon olefin Download PDFInfo
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- CN101333141A CN101333141A CNA2008100436138A CN200810043613A CN101333141A CN 101333141 A CN101333141 A CN 101333141A CN A2008100436138 A CNA2008100436138 A CN A2008100436138A CN 200810043613 A CN200810043613 A CN 200810043613A CN 101333141 A CN101333141 A CN 101333141A
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Abstract
The invention relates to a reaction device which uses methanol or dimethyl ether to prepare low-carbon olefin, mainly to solve the problem of low low-carbon olefin production rate in the prior art. The reaction device which uses methanol or dimethyl ether to prepare low-carbon olefin mainly comprises a reactor reaction zone 2, a catalyst circulation zone, a stripping zone 4, a reactor separation zone 9, a regenerator regeneration zone 14 and a regenerator separation zone 12; a material inlet 1 is arranged at the lower part of the reactor reaction zone 2; the upper part of the reactor reaction zone is connected with a gas-solid rapid separation equipment 3; a gas-solid cyclone separator 8 is arranged inside the reactor separation zone 9; the upper part of the reactor separation zone 9 is provided with a product outlet 11; the stripping zone 4 is arranged at the upper part of the reactor reaction zone 2; two catalyst outlets are arranged at the lower part of the reactor reaction zone 2, wherein, one catalyst outlet is connected with the reactor reaction zone 2, while the other catalyst outlet is connected with the regenerator regeneration zone 14; a gas-solid cyclone separator 16 is arranged inside the regenerator separation zone 12; a flue gas outlet 17 is arranged at the upper part of the regenerator separation zone 12; a catalyst outlet is arranged at the upper part of the regenerator regeneration zone 14 and connected with a regenerated catalyst standpipe 21; the opening of the regenerated catalyst standpipe 21 is connected with the stripping zone 4. Such a technical proposal solves all the problems and the device can be used for low-carbon olefin industrial production.
Description
Technical field
The present invention relates to the reaction unit that a kind of methyl alcohol or dimethyl ether conversion are 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.
Known in the field, guarantee high selectivity of light olefin, need the carbon distribution of some amount on the catalyzer, and methyl alcohol or dimethyl ether conversion are very responsive to processing parameters such as temperature of reaction in the process of low-carbon alkene.All there are problems such as the fluctuation of reaction zone inner catalyst carbon deposit skewness, temperature of reaction is big in prior art.The present invention has solved this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the not high problem of yield of light olefins that exists in the prior art, and it is the reaction unit of low-carbon alkene that a kind of new methyl alcohol or dimethyl ether conversion are provided.This method is used for the production of low-carbon alkene, has that yield of light olefins is higher, the advantage of low-carbon alkene production technique better economy.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of methyl alcohol or dimethyl ether conversion are the reaction unit of low-carbon alkene, mainly comprise reactor reaction zone 2, catalyst recirculation district, stripping zone 4, reactor disengaging zone 9, revivifier breeding blanket 14, revivifier disengaging zone 12; Reactor reaction zone 2 bottoms have opening for feed 1, and top links to each other with gas-solid sharp separation equipment 3, and 9 inside, reactor disengaging zone are provided with gas-solid cyclone separator 8, and top has products export 11; Stripping zone 4 is positioned at reactor reaction zone 2 tops, and the bottom has two catalyst outlets, and one links to each other with reactor reaction zone 2, and another links to each other with revivifier breeding blanket 14; 12 inside, revivifier disengaging zone are provided with gas-solid cyclone separator 16, and top has exhanst gas outlet 17; 14 tops, revivifier breeding blanket have catalyst outlet, link to each other with regenerated catalyst standpipe 21, and regenerated catalyst standpipe 21 outlets link to each other with stripping zone 4.
In the technique scheme, described reactor is a fast fluidized bed; The diameter of gas-solid sharp separation equipment 3 and the diameter ratio of reactor reaction zone 2 are 0.1～0.5: 1; Gas-solid cyclone separator 8 in the reactor disengaging zone 9 is 1～3 grade; Gas-solid cyclone separator 16 in the revivifier disengaging zone 12 is 1～3 grade; Lifting medium in the regeneration standpipe 21 is water vapour, unreacted methanol or dme, carbon four above hydrocarbon; Catalyzer comprises the SAPO-34 molecular sieve; Revivifier external warmer 15 is the back-mixing formula.
Because oxygenate is in the reaction process of low-carbon alkene, needs to be with on the catalyzer a certain amount of carbon, to improve the selectivity of low-carbon alkene.General, adopt with reclaimable catalyst and regenerated catalyst blended method, to reach required coke content requirement.And more importantly be that before mixed catalyst contact raw material, catalyzer requires to mix, and could realize maximized selectivity requirement.Known in the field, in the existing circulating fluidized bed technique, as fluid catalytic cracking (FCC), be regenerated catalyst directly to be turned back to riser reaction zone contact with raw material, but, do not relate to the mixed problem of different carbon-bearing amount catalyzer because prior art generally all requires the mean carbon content of reaction zone catalyzer low more good more.In addition, because oxygenate is that the reaction of low-carbon alkene is very responsive for temperature of reaction, the fluctuation of reaction zone temperature of reaction will directly influence reaction effect, if the higher regenerated catalyst of temperature directly turns back to reaction zone, will certainly influence the temperature of reaction of reaction zone.Therefore, generally speaking, be in the process of low-carbon alkene in oxygenate, the solid flow of regenerated catalyst line mainly plays two effects: the one, control suitable flow and mix with reclaimable catalyst, reach the required average coke content of catalyzer; The 2nd, control suitable flow and enter reaction zone, guarantee the stable of heat that reaction zone is required and temperature of reaction.And in the prior art, above-mentioned two effects tend to produce contradiction, as: the regenerated catalyst flow is big, the heat height that obtains of reaction zone then, temperature of reaction raises, but owing to the ratio of regenerated catalyst in the mixed catalyst increases, has then reduced the average coke content of mixed catalyst.Adopt method of the present invention, regenerated catalyst is turned back to stripping zone by the catalyzer standpipe, and, reduced the temperature of regenerated catalyst simultaneously, effectively solved the problems referred to above the mixing region of stripping zone as catalyzer.
Therefore, adopt method of the present invention, regenerated catalyst risen to the disengaging zone of reactor by promoting medium so that and reclaimable catalyst mix, can also reach the effect that influences the reaction zone operating parameters that minimizes.In addition, because methyl alcohol or dimethyl ether conversion are in the reaction process of low-carbon alkene, can there be unreacted methanol or dme, and can produce the above hydrocarbon of the lower C4 of a certain amount of added value, if the above hydrocarbon of C4 in unreacted methanol or dme or the product is contacted with regenerated catalyst as promoting medium, not only can generate low-carbon alkene, improved the utilising efficiency of methyl alcohol or dme or the above hydrocarbon of C4, but also regenerated catalyst has been carried out pre-coking, thereby the carbon that dwindles reclaimable catalyst and regenerated catalyst is poor.When the average coke content one of reaction zone mixed catalyst regularly because the carbon difference of reclaimable catalyst and regenerated catalyst is less, catalyst carbon deposit narrow distribution then, thereby improved the selectivity of low-carbon alkene greatly.In addition, because dwindling of reclaimable catalyst and regenerated catalyst carbon difference can be adopted bigger catalyst recirculation amount operation between reaction and regeneration system rapidly, be easy to control more.
Adopt technical scheme of the present invention: described reactor is a fast fluidized bed; The diameter of gas-solid sharp separation equipment 3 and the diameter ratio of reactor reaction zone 2 are 0.1～0.5: 1; Gas-solid cyclone separator 8 in the reactor disengaging zone 9 is 1～3 grade; Gas-solid cyclone separator 16 in the revivifier disengaging zone 12 is 1～3 grade; Lifting medium in the regeneration standpipe 21 is water vapour, unreacted methanol or dme, carbon four above hydrocarbon; Catalyzer comprises the SAPO-34 molecular sieve; Revivifier external warmer 15 is the back-mixing formula, and selectivity of light olefin can reach 83.67% 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 reactor feedstocks charging; 2 is reactor reaction zone; 3 are gas-solid sharp separation equipment; 4 is stripping zone; 5 is reclaimable catalyst circulation inclined tube; 6 remove the revivifier line of pipes for reclaimable catalyst; 7 is the reactor external warmer; 8 is the reactor gas-solid cyclone separator; 9 is the reactor disengaging zone; 10 is the product collection chamber; 11 is the product gas outlet pipeline; 12 is the revivifier disengaging zone; 13 is the regenerating medium source line; 14 is the revivifier breeding blanket; 15 is the revivifier external warmer; 16 is the revivifier gas-solid cyclone separator; 17 is the regenerated flue gas outlet line; 18 is regenerated catalyst circulation inclined tube; 19 are regenerated catalyst standpipe lifting medium inlet pipeline; 20 is the mixing section of regenerated catalyst standpipe bottom; 21 is regenerated catalyst standpipe; 22 gas-solid cyclone separators for the regenerated catalyst standpipe outlet.
Oxygen-containing compound material enters in the reactor reaction zone 2 through feeding line 1, contacts with molecular sieve catalyst, and reaction is given birth to Become to contain the product of low-carbon alkene, carry reclaimable catalyst and enter the reactor Disengagement zone through the quick separation equipment 3 of gas-solid, its In, most of catalyst that the quick separation equipment 3 of gas-solid is separated enters stripping zone 4, and gaseous products and part are not The catalyst that is separated by the quick separation equipment of gas-solid carries out Re-isolation through entering cyclone separator 8 separation, and catalyst is through whirlwind The dipleg of separator 8 turns back to stripping zone 4, and gaseous products enters collection chamber 10 and enters follow-up branch by outlet line 11 From workshop section. Be divided into two ones by the quick separation equipment 3 of gas-solid and cyclone separator 8 isolated reclaimable catalysts through behind the stripping Divide, turn back to the bottom of reactor reaction zone 2 after 7 heat exchange of part process heat exchanger by catalyst circulation inclined tube 5, in addition An outer part enters coke-burning regeneration in the regenerator renewing zone 14 through catalyst transport pipeline 6, the flue gas that the coke burning generates Through entering follow-up energy-recuperation system by exhanst gas outlet pipeline 17 behind the cyclone separator 16, the catalyst that regeneration is finished Enter by regenerated catalyst circulation inclined tube 18 in the mixing section 20 of catalyst standpipe 21 bottoms, mix with lifting medium 19, The regenerated catalyst standpipe outlet is provided with gas-solid cyclone separator 22, and isolated regenerated catalyst enters in the stripping zone 4 with to be generated Catalyst mix, part turns back to sustainable participation reaction in the reaction zone 2 through circulation inclined tube 5.
The invention will be further elaborated below by embodiment, but be not limited only to present embodiment.
Embodiment
[embodiment 1]
In the fast fluidized bed reaction unit, the same Fig. 1 of reaction unit pattern.The medial temperature of reactor reaction zone 2 is 470 ℃, the medial temperature of revivifier breeding blanket 14 is 650 ℃, reactor disengaging zone 9 top pressures are counted 0.14MPa with gauge pressure, pure methanol feeding, charging is 2 kilograms/hour, and catalyzer is a modified SAPO-34, and stripping zone 4 stripping media are water vapour, the lifting medium of regenerated catalyst standpipe 21 is unreacted methanol and dme, and the heat transferring medium with reclaimable catalyst in the reactor external warmer 7 is a water vapour.The diameter of gas-solid sharp separation equipment 3 and the diameter ratio of reactor reaction zone 2 are 0.2: 1; Gas-solid cyclone separator 8 in the reactor disengaging zone 9 is 2 grades; Gas-solid cyclone separator 16 in the revivifier disengaging zone 12 is 2 grades; Revivifier external warmer 15 is the back-mixing formula.Average catalyst coke content in the reactor reaction zone 2 is controlled at about 3% weight, keeps the stability of catalyst flow control, the reactor outlet product adopts online gas chromatographic analysis, and yield of light olefins reaches 81.04% weight.
[embodiment 2]
According to embodiment 1 described condition, it is the above hydrocarbon of the isolated C4 of product separation workshop section that regenerated catalyst standpipe promotes medium, the medial temperature that changes reactor reaction zone 2 is 500 ℃, and the diameter of gas-solid sharp separation equipment 3 and the diameter ratio of reactor reaction zone 2 are 0.5: 1; Gas-solid cyclone separator 8 in the reactor disengaging zone 9 is 3 grades; Gas-solid cyclone separator 16 in the revivifier disengaging zone 12 is 1 grade, and yield of light olefins reaches 83.67% weight.
[embodiment 3]
According to embodiment 1 described condition, it is water vapour that regenerated catalyst standpipe promotes medium, and the medial temperature that changes reactor reaction zone 2 is 450 ℃, and the diameter of gas-solid sharp separation equipment 3 and the diameter ratio of reactor reaction zone 2 are 0.1: 1; Gas-solid cyclone separator 8 in the reactor disengaging zone 9 is 1 grade; Gas-solid cyclone separator 16 in the revivifier disengaging zone 12 is 3 grades, and yield of light olefins reaches 80.01% weight.
[comparative example 1]
According to embodiment 1 described condition, regenerated catalyst is directly turned back to the bottom of reactor reaction zone 2 by regenerated catalyst circulation inclined tube 18, yield of light olefins is 78.28% weight.
Obviously, adopt method of the present invention, can reach the purpose that improves yield of light olefins, have bigger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (6)
1, a kind of methyl alcohol or dimethyl ether conversion are the reaction unit of low-carbon alkene, mainly comprise reactor reaction zone (2), catalyst recirculation district, stripping zone (4), reactor disengaging zone (9), revivifier breeding blanket (14), revivifier disengaging zone (12); Reactor reaction zone (2) bottom has opening for feed (1), and top links to each other with gas-solid sharp separation equipment (3), and inside, reactor disengaging zone (9) is provided with gas-solid cyclone separator (8), and top has products export (11); Stripping zone (4) is positioned at reactor reaction zone (2) top, and the bottom has two catalyst outlets, and one links to each other with reactor reaction zone (2), and another links to each other with revivifier breeding blanket (14); Inside, revivifier disengaging zone (12) is provided with gas-solid cyclone separator (16), and top has exhanst gas outlet (17); Top, revivifier breeding blanket (14) has catalyst outlet, links to each other with regenerated catalyst standpipe (21), and regenerated catalyst standpipe (21) outlet links to each other with stripping zone (4).
2, be the reaction unit of low-carbon alkene according to described methyl alcohol of claim 1 or dimethyl ether conversion, it is characterized in that described reactor is a fast fluidized bed; The diameter ratio of the diameter of gas-solid sharp separation equipment (3) and reactor reaction zone (2) is 0.1～0.5: 1.
3, be the reaction unit of low-carbon alkene according to described methyl alcohol of claim 2 or dimethyl ether conversion, it is characterized in that the gas-solid cyclone separator (8) in the described reactor disengaging zone (9) is 1～3 grade; Gas-solid cyclone separator (16) in the revivifier disengaging zone (12) is 1～3 grade.
4, be the reaction unit of low-carbon alkene according to described methyl alcohol of claim 1 or dimethyl ether conversion, it is characterized in that the lifting medium in the described regeneration standpipe (21) is water vapour, unreacted methanol or dme, carbon four above hydrocarbon.
5, be the reaction unit of low-carbon alkene according to described methyl alcohol of claim 1 or dimethyl ether conversion, it is characterized in that described catalyzer comprises the SAPO-34 molecular sieve.
6, be the reaction unit of low-carbon alkene according to described methyl alcohol of claim 1 or dimethyl ether conversion, it is characterized in that described revivifier external warmer (15) is the back-mixing formula.
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| CN102190548A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Method for enhancing yield of light olefins in MTO technology |
| CN102190540A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Method for producing propylene |
| CN102276406A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Method for increasing yield of propylene |
| CN102276383A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Method of reducing runoff of catalysts in conversion of oxygen containing compounds to low carbon olefins |
| CN102276381A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Method for improving selectivity of light olefins prepared from conversion of oxygenated compound |
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| CN102463072A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Reaction device for producing p-xylene |
| CN102659499A (en) * | 2012-05-14 | 2012-09-12 | 神华集团有限责任公司 | Device and method for converting methyl alcohol into low-carbon olefin |
| CN102875290A (en) * | 2011-07-12 | 2013-01-16 | 中国石油化工股份有限公司 | Reaction unit for preparing low-carbon olefins by using methanol and naphtha |
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| US9212105B2 (en) | 2010-03-03 | 2015-12-15 | Shanghai Research Institute Of Petrochemical Technology, Sinopec | Processes for producing at least one light olefin |
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| CN102190548B (en) * | 2010-03-03 | 2014-07-02 | 中国石油化工股份有限公司 | Method for enhancing yield of light olefins in MTO technology |
| US9212105B2 (en) | 2010-03-03 | 2015-12-15 | Shanghai Research Institute Of Petrochemical Technology, Sinopec | Processes for producing at least one light olefin |
| CN102276383A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Method of reducing runoff of catalysts in conversion of oxygen containing compounds to low carbon olefins |
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| US9295963B2 (en) | 2010-11-17 | 2016-03-29 | China Petroleum & Chemical Corporation | Processes for producing light olefins |
| CN102872907A (en) * | 2011-07-12 | 2013-01-16 | 中国石油化工股份有限公司 | Regenerator for preparing olefins from methanol |
| CN102875290A (en) * | 2011-07-12 | 2013-01-16 | 中国石油化工股份有限公司 | Reaction unit for preparing low-carbon olefins by using methanol and naphtha |
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| CN102659499B (en) * | 2012-05-14 | 2014-08-27 | 神华集团有限责任公司 | Device and method for converting methyl alcohol into low-carbon olefin |
| CN102659499A (en) * | 2012-05-14 | 2012-09-12 | 神华集团有限责任公司 | Device and method for converting methyl alcohol into low-carbon olefin |
| CN115155466A (en) * | 2022-08-05 | 2022-10-11 | 中国石油大学(北京) | Coupling reaction system and method for preparing ethylene through oxidative coupling of methane |
| CN115155466B (en) * | 2022-08-05 | 2023-10-13 | 中国石油大学(北京) | Coupling reaction system and method for preparing ethylene by oxidative coupling of methane |
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