CN101402538A - Method for improving yield of light olefins - Google Patents
Method for improving yield of light olefins Download PDFInfo
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- CN101402538A CN101402538A CNA2008100439719A CN200810043971A CN101402538A CN 101402538 A CN101402538 A CN 101402538A CN A2008100439719 A CNA2008100439719 A CN A2008100439719A CN 200810043971 A CN200810043971 A CN 200810043971A CN 101402538 A CN101402538 A CN 101402538A
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Abstract
The invention relates to a method for improving the yield of low-carbon olefin, which mainly solves the problem that the yield of the low-carbon olefin in the prior art is low. The invention discloses the method for improving the yield of the low-carbon olefin, which mainly comprises the following steps: (1) providing a fluidized bed reactor comprising a first reaction zone, a second reaction zone, a gas-solid separation zone, a catalyst steam stripping zone, and a catalyst circulation zone; (2) putting a raw material with methanol into the first reaction zone to contact a molecular sieve catalyst so as to produce a product with the low-carbon olefin which enters the second reaction zone along with the catalyst to contact a regenerated catalyst from a regenerator so as to produce a product substance flow with higher content of the low-carbon olefin; and (3) separating the product substance flow with the higher content of the low-carbon olefin and the catalyst, putting the product substance flow with the higher content of the low-carbon olefin into a separating section, performing steam stripping on the separated catalyst and putting part of the catalyst into the regenerator for regeneration, wherein part of the catalyst recycles back to the first reaction zone, thus the technical proposal solves the problems better and can be used in the industrial production of the low-carbon olefin.
Description
Technical field
The present invention relates to a kind of method that improves yield of light olefins.
Background technology
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 methanol conversion is 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.In addition, prepare in the process of low-carbon alkene, inevitably can produce some by product,,, will improve the yield and the process economy of low-carbon alkene if these by products further are converted into the purpose product as carbon four above hydrocarbon etc. at methyl alcohol.The present invention has solved the problems referred to above 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 a kind of method of new raising yield of light olefins is 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 method that improves yield of light olefins, mainly may further comprise the steps: (1) provides a kind of fluidized bed reaction, comprise first reaction zone, second reaction zone, gas solid separation district, catalyst stripping district, catalyst recirculation district: (2) comprise that the raw material of methyl alcohol enters first reaction zone and contacts with molecular sieve catalyst, generation comprises the product of low-carbon alkene, enter second reaction zone with catalyzer, contact with the regenerated catalyst that comes from revivifier, generate the higher product stream of low-carbon alkene content; (3) enter centrifugal station after product stream that described low-carbon alkene content is higher and the catalyst separating, isolated catalyzer behind stripping wherein a part go revivifier regeneration, wherein first reaction zone is returned in part circulation.
In the technique scheme, gas void tower linear speed is at 0.6～2.0 meter per second in described first reaction zone, and the diameter ratio of second reaction zone and first reaction zone is 1.1～2.0: 1; The diameter of gas-solid sharp separation equipment and the diameter ratio of second reaction zone are 0.1～0.5: 1; Going revivifier regenerated catalyzer and the weight ratio of returning the catalyzer of first reaction zone is 0.1～2.0: 1; The described second reaction zone inside can be provided with interior heat collector; Lifting medium in the described regenerated catalyst circulation tube comprises water vapour, unreacted methanol, dme or carbon four above hydrocarbon; Described catalyzer comprises the SAPO-34 molecular sieve; The described second reaction zone axial location is provided with opening for feed, and charging comprises unreacted methanol, dme or carbon four above hydrocarbon; The temperature of reaction of described first reaction zone is 400～500 ℃, and bed density is 50～200 kilograms per cubic meter, and the average coke content of catalyzer is 2～3.5% weight; The temperature of reaction of second reaction zone is 480～600 ℃, and bed density is 150～300 kilograms per cubic meter; Between described first reaction zone and second reaction zone grid distributor is set, percentage of open area is 0.8～2%; On the described pipeline that returns first reaction zone at catalyzer external warmer is set.
The method of the invention has the following advantages: in the product of (1) first reaction zone outlet, as carbon four above hydrocarbon, unreacted methanol or dme etc., can continue reaction at second reaction zone, generate low-carbon alkene, improve purpose product yield and feed stock conversion; Parameters such as the material level of (2) second reaction zones, temperature of reaction can independently be controlled, to guarantee the changing effect of second reaction zone; (3) the pyritous regenerated catalyst turns back to second reaction zone, helps the conversion of carbon four above hydrocarbon to low-carbon alkene, has replenished the heat of second reaction zone, and has reduced the influence of regenerated catalyst to first reaction zone; (4) regenerated catalyst turns back to second reaction zone, can accumulate a certain amount of carbon deposit after the reaction, returns first reaction zone then, has improved the selectivity of light olefin in first reaction zone; (5) second reaction zone tops are provided with gas-solid sharp separation equipment, have shortened the residence time of purpose product, the generation that has alleviated secondary reaction; (6) second reaction zone diameter are slightly larger than first reaction zone diameter, have guaranteed the required residence time of the second reaction zone internal reaction; (7) second reaction zones are axially arranged with opening for feed, can improve total conversion rate and purpose product yield with returning second reaction zone after unreacted carbon four above hydrocarbon or the separation such as methyl alcohol, dme.
Adopt technical scheme of the present invention: gas void tower linear speed is at 0.6～2.0 meter per second in described first reaction zone, and the diameter ratio of second reaction zone and first reaction zone is 1.1～2.0: 1; The diameter of gas-solid sharp separation equipment and the diameter ratio of second reaction zone are 0.1～0.5: 1; Going revivifier regenerated catalyzer and the weight ratio of returning the catalyzer of first reaction zone is 0.1～2.0: 1; The described second reaction zone inside can be provided with interior heat collector; Lifting medium in the described regenerated catalyst circulation tube comprises water vapour, unreacted methanol, dme or carbon four above hydrocarbon; Described catalyzer comprises the SAPO-34 molecular sieve; The described second reaction zone axial location is provided with opening for feed, and charging comprises unreacted methanol, dme or carbon four above hydrocarbon; The temperature of reaction of described first reaction zone is 400～500 ℃, and bed density is 50～200 kilograms per cubic meter, and the average coke content of catalyzer is 2～3.5% weight; The temperature of reaction of second reaction zone is 480～600 ℃, and bed density is 150～300 kilograms per cubic meter; Between described first reaction zone and second reaction zone grid distributor is set, percentage of open area is 0.8～2%; On the described pipeline that returns first reaction zone at catalyzer external warmer is set, selectivity of light olefin can reach 88.43% 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 first reaction zone; 3 is second reaction zone; 4 is second reaction zone bottom grid distributor; 5 are gas-solid sharp separation equipment; 6 is gas-solid cyclone separator; 7 is the reactor disengaging zone; 8 is the reactor product outlet line; 9 is the reclaimable catalyst inclined tube; 10 is the external warmer inclined tube; 11 is the reactor external warmer; 12 is the second reaction zone axial location opening for feed; 13 is reactor outer circulation inclined tube; 14 are regenerated catalyst circulation tube lifting medium inlet; 15 is the regenerated catalyst circulation tube.
Raw material enters in first reaction zone 2 through feeding line 1, contacts with molecular sieve catalyst, and reaction generates and contains low carbene The product of hydrocarbon enters second reaction zone through behind the distribution grid 4, contacts with regenerated catalyst and continue to react reacted product Thing enters the quick separation equipment 5 of gas-solid, and most of catalyst is separated and enters the bottom in gas solid separation district 7, and gas phase Product and part are not carried out Re-isolation by the catalyst that the quick separation equipment 5 of gas-solid separates through entering cyclone separator 6, urge The dipleg of changing agent process cyclone separator 6 turns back to the bottom in gas solid separation district 7, and gaseous products is after outlet line 8 enters Continuous centrifugal station. Divided through behind the stripping by the quick separation equipment 5 of gas-solid and cyclone separator 6 isolated reclaimable catalysts Be three parts, turn back to first reaction zone 2 after 11 heat exchange of part process reactor external warmer, a part is through to be generated urging Change agent inclined tube 9 and enter coke-burning regeneration in the regenerator, a part is returned first reaction zone 2 through reactor outer circulating tube 13 in addition; The catalyst that regeneration is finished enters the reaction of second reaction zone 3 sustainable participations by regenerated catalyst circulation pipe 14.
The invention will be further elaborated below by embodiment, but be not limited only to present embodiment.
Embodiment
[embodiment 1]
In reaction unit as shown in Figure 1, the medial temperature of first reaction zone 2 is 470 ℃, and bed density is 80 kilograms per cubic meter, and the medial temperature of second reaction zone 3 is 530 ℃, and bed density is 200 kilograms per cubic meter.Reactor disengaging zone 7 top pressures are counted 0.14MPa with gauge pressure, pure methanol feeding, charging is 2 kilograms/hour, gas void tower linear speed is at 1.1 meter per seconds in first reaction zone 2, catalyzer is a modified SAPO-34, the lifting medium of regenerated catalyst circulation tube 15 is unreacted methanol and dme, and the heat transferring medium with reclaimable catalyst in the reactor external warmer 11 is a water vapour.The diameter ratio of second reaction zone 3 and first reaction zone 2 is 1.2: 1; The diameter of gas-solid sharp separation equipment 5 and the diameter ratio of second reaction zone 3 are 0.3: 1.Going revivifier regenerated catalyzer and the weight ratio of returning the catalyzer of first reaction zone is 0.1: 1.Heat collector in the coil tube type is set in second reaction zone 3, and the bottom is provided with grid distributor, and percentage of open area is 1.2%.The charging medium of second district's axial feed inlet 12 is the isolated carbon four above hydrocarbon of product separation workshop section, and inlet amount is 10% weight of methanol feeding amount.Average catalyst coke content in first 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 87.44% weight.
[embodiment 2]
According to embodiment 1 described condition, the medial temperature of first reaction zone 2 is 500 ℃, bed density is 50 kilograms per cubic meter, gas void tower linear speed is at 2.0 meter per seconds, average catalyst coke content in first reaction zone 2 is controlled at about 2% weight, the medial temperature of second reaction zone 3 is 600 ℃, bed density is 150 kilograms per cubic meter, the diameter ratio of second reaction zone 3 and first reaction zone 2 is 2.0: 1, and the diameter of gas-solid sharp separation equipment 5 and the diameter ratio of second reaction zone 3 are 0.1: 1.Going revivifier regenerated catalyzer and the weight ratio of returning the catalyzer of first reaction zone is 2.0: 1.The lifting medium of regenerated catalyst circulation tube 15 is a water vapour, and second reaction zone, 3 bottom grid distributor percentage of open area are 0.8%.The charging medium of second district's axial feed inlet 12 is the dme of unreacted methanol and generation.Yield of light olefins reaches 84.11% weight.
[embodiment 3]
According to embodiment 1 described condition, the product separation workshop section above hydrocarbon of isolated C4 is divided into two portions, a part is used as the lifting medium of regenerated catalyst circulation tube 15, a part enters second reaction zone by the opening for feed on second reaction zone, 3 axial locations, the opening for feed number is two, for to the spray formula, the distance of opening for feed position range distribution plate 4 is 1/4 of second reaction zone, 3 height.The medial temperature that changes first reaction zone 2 is 500 ℃, and the diameter ratio of second reaction zone 3 and first reaction zone 2 is 1.4: 1; The diameter of gas-solid sharp separation equipment 5 and the diameter ratio of second reaction zone 3 are 0.5: 1, and yield of light olefins reaches 88.43% weight.
[embodiment 4]
According to embodiment 1 described condition, the medial temperature of first reaction zone 2 is 400 ℃, bed density is 200 kilograms per cubic meter, gas void tower linear speed is at 0.6 meter per second, average catalyst coke content in first reaction zone 2 is controlled at about 3.5% weight, the medial temperature of second reaction zone 3 is 480 ℃, bed density is 300 kilograms per cubic meter, the diameter ratio of second reaction zone 3 and first reaction zone 2 is 2.0: 1, the diameter of gas-solid sharp separation equipment 5 and the diameter ratio of second reaction zone 3 are 0.3: 1, the lifting medium of regenerated catalyst circulation tube 15 is a water vapour, and second reaction zone, 3 bottom grid distributor percentage of open area are 2%.The charging medium of second district's axial feed inlet 12 is the dme of unreacted methanol and generation.Yield of light olefins reaches 85.71% weight.
[comparative example 1]
According to embodiment 1 described condition, do not establish second reaction zone 3, regenerated catalyst directly turns back to the bottom of first reaction zone 2, and low-carbon alkene carbon back yield is 78.15% 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 (9)
1, a kind of method that improves yield of light olefins mainly may further comprise the steps:
(1) provide a kind of fluidized bed reaction, comprise first reaction zone, second reaction zone, gas solid separation district, catalyst stripping district, catalyst recirculation district:
(2) raw material that comprises methyl alcohol enters first reaction zone and contacts with molecular sieve catalyst, generates the product that comprises low-carbon alkene, enters second reaction zone with catalyzer, contact the higher product stream of generation low-carbon alkene content with the regenerated catalyst that comes from revivifier;
(3) enter centrifugal station after product stream that described low-carbon alkene content is higher and the catalyst separating, isolated catalyzer behind stripping wherein a part go revivifier regeneration, wherein first reaction zone is returned in part circulation.
2, according to the method for the described raising yield of light olefins of claim 1, it is characterized in that gas void tower linear speed is at 0.6～2.0 meter per second in described first reaction zone, the diameter ratio of second reaction zone and first reaction zone is 1.1～2.0: 1; The diameter of gas-solid sharp separation equipment and the diameter ratio of second reaction zone are 0.1～0.5: 1; Going revivifier regenerated catalyzer and the weight ratio of returning the catalyzer of first reaction zone is 0.1～2.0: 1.
3,, it is characterized in that the described second reaction zone inside can be provided with interior heat collector according to the method for the described raising yield of light olefins of claim 1.
4,, it is characterized in that the lifting medium in the described regenerated catalyst circulation tube comprises water vapour, unreacted methanol, dme or carbon four above hydrocarbon according to the method for the described raising yield of light olefins of claim 1.
5,, it is characterized in that described catalyzer comprises the SAPO-34 molecular sieve according to the method for the described raising yield of light olefins of claim 1.
6, according to the method for the described raising yield of light olefins of claim 1, it is characterized in that the described second reaction zone axial location is provided with opening for feed, charging comprises unreacted methanol, dme or carbon four above hydrocarbon.
7, according to the method for the described raising yield of light olefins of claim 1, the temperature of reaction that it is characterized in that described first reaction zone is 400～500 ℃, bed density is 50～200 kilograms per cubic meter, the average coke content of catalyzer is 2～3.5% weight, the temperature of reaction of second reaction zone is 480～600 ℃, and bed density is 150～300 kilograms per cubic meter.
8, according to the method for the described raising yield of light olefins of claim 1, it is characterized in that between described first reaction zone and second reaction zone grid distributor being set, percentage of open area is 0.8～2%.
9,, it is characterized in that on the described pipeline that returns first reaction zone at catalyzer external warmer being set according to the method for the described raising yield of light olefins of claim 1.
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