CN102276381B - Method for improving selectivity of light olefins prepared from conversion of oxygenated compound - Google Patents
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Abstract
The invention relates to a method for improving selectivity of light olefins prepared from conversion of an oxygenated compound, and a purpose of the present invention is mainly to solve the problem of poor average carbon deposition level of a catalyst in a reactor in the prior art. According to the present invention, the method for improving the selectivity of the light olefins prepared from conversion of the oxygenated compound is adopted. The method mainly comprises the following steps that: a) raw materials of the oxygenated compound contact a molecular sieve catalyst in a fluidized bed reactor to generate product stream I containing the light olefins and the carbon deposited catalyst; b) the product stream I is subjected to gas-solid separation, then the gas-phase product containing the light olefins flows from the top of the reactor, and the solid-phase carbon deposited catalyst enters the sedimentation segment of the reactor; c) the carbon deposited catalyst in the sedimentation segment of the reactor is divided into at least two parts, wherein the first part enters the reactor through a circulating pipeline of the reactor, the second part enters a regenerator through a spent pipeline; d) the carbon deposited catalyst is regenerated through the regenerator, and then enters the sedimentation segment of the regenerator to ensure the height of the catalyst bed in the sedimentation segment of the regenerator, such that the catalyst can naturally flow in the sedimentation segment of the reactor after steam stripping; e) one part of the catalyst in the sedimentation segment of the regenerator returns to the regenerator through a circulating pipeline of the regenerator. With the technical scheme of the present invention, the regenerator is adopted as the lift pipe, such that the problem in the prior art is solved better; the method can be applicable for the industrial production of the light olefins prepared through conversion of the oxygenated compound.
Description
Technical field
The present invention relates to a kind of optionally method of raising converting oxygen-containing compound to low-carbon olefins.
Background technology
Low-carbon alkene, is defined as ethene and propylene here, is two kinds of important basic chemical industry raw materials, and its demand is in continuous increase.Ethene, propylene are mainly to make by petroleum path traditionally, but due to the limited supply of petroleum resources and higher price, the cost of being produced ethene, propylene by petroleum resources constantly increases.In recent years, people start to greatly develop substitute energy transformation technology, and as the technique of oxygen-containing compound conversion to produce olefine (OTO), oxygenatedchemicals comprises methyl alcohol, ethanol, dme, methyl ethyl ether, methylcarbonate etc.Have many technology to can be used to produce oxygenatedchemicals, raw material comprises coal, Sweet natural gas, biomass etc.As methyl alcohol, can be made by coal or Sweet natural gas, technique is very ripe, can realize the industrial scale of up to a million tonnes.Popularity due to oxygenatedchemicals source, add and transform the economy that generates low-carbon alkene technique, so by the technique of oxygen-containing compound conversion to produce olefine (OTO), particularly the technique by preparing olefin by conversion of methanol (MTO) is subject to increasing attention.
In US4499327 patent, silicoaluminophosphamolecular molecular sieve catalyst is applied to preparing olefin by conversion of methanol technique and studies in detail, think that SAPO-34 is the first-selected catalyzer of MTO technique.SAPO-34 catalyzer has very high selectivity of light olefin, and activity is also higher, and can make methanol conversion is reaction times of low-carbon alkene to be less than the degree of 10 seconds, more even reaches in the reaction time range of riser tube.
For MTO technology, on SAPO-34 catalyzer, long-pending a certain amount of carbon can effectively improve the selectivity of low-carbon alkene in reaction product, and has a best catalyst carbon deposit weight range to make the selectivity of low-carbon alkene the highest.Therefore, control certain coke content by entering on the catalyzer of reactor, and then reach and control compared with the object of high-low carbon olefine selective.In addition, for having the catalyzer of best coke content, the carbon deposit on granules of catalyst is average, and in product, the selectivity of low-carbon alkene is just higher.Therefore it is crucial, in MTO technology, how the catalyzer coke content in reaction zone being evenly controlled to certain level.
The method that relates to catalyzer coke content in a kind of MTO of control reactor reaction zone in US20060025646 patent, is a catalyzer part for inactivation to be sent into breeding blanket make charcoal, and another part decaying catalyst turns back to reaction zone and continues reaction.
The carbon that can make in aforesaid method to enter between two strands of catalyzer in reactor is poor very large, and the catalyzer that contains more carbon and the catalyzer that contains carbon are seldom all unfavorable to the selectivity of low-carbon alkene, cause the problem that the fluctuation of low-carbon alkene selectivity of product is large, object selectivity of product is lower.
Summary of the invention
Technical problem to be solved by this invention is in prior art, to have the not good problem of the average carbon deposit level of catalyst in reactor, and a kind of optionally method of new raising converting oxygen-containing compound to low-carbon olefins is provided.The method is for the production of low-carbon alkene, has advantages of that catalyst in reactor carbon deposit is average, selectivity of light olefin is higher in product.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows, a kind of raising converting oxygen-containing compound to low-carbon olefins is method optionally, mainly comprise the following steps: a) raw material of oxygenatedchemicals contacts with molecular sieve catalyst in fluidized-bed reactor, generate the product logistics I that comprises low-carbon alkene and carbon deposited catalyst; B) logistics I is after gas solid separation, and the gas-phase product that contains low-carbon alkene flows out from reactor head, and its solid phase carbon deposited catalyst enters reactor settling section; C) in reactor settling section, carbon deposited catalyst is at least divided into two portions, and first part enters reactor through reactor cycles pipeline, and second section enters revivifier through pipeline to be generated; D) carbon deposited catalyst enters revivifier settling section after revivifier regeneration, guarantees that revivifier settling section inner catalyst bed height makes catalyzer after stripping, naturally flow into reactor settling section; E) in revivifier settling section, a part of catalyzer returns to revivifier through revivifier circulation line; Wherein, revivifier is riser tube.
In technique scheme, the oxygenatedchemicals in raw material is at least one in methyl alcohol or dme, and described molecular sieve catalyst is selected from SAPO type molecular sieve.Oxygenatedchemicals in raw material is preferably methyl alcohol, and SAPO type molecular screening is from SAPO-34 molecular sieve.The temperature of reactor is 350～600 ℃, and the pressure in reactor is counted 0～1MPa with gauge pressure, and raw material weight air speed is 0.1～20 hour
-1between; Temperature in revivifier is between 550～700 ℃, in revivifier, take gauge pressure pressure as 0～1MPa.The temperature of reactor is preferably 420～500 ℃, and the pressure in reactor is preferably 0.1～0.3MPa in gauge pressure, and raw material weight air speed is preferably 3～8 hours
-1; Temperature in revivifier is preferably 600～650 ℃, in revivifier, in gauge pressure pressure, is preferably 0.1～0.3MPa.Carbon deposition catalyst is in mass flux ratio first part in settling section: second section=1: 0.01～2; Carbon deposition catalyst is in the preferred first part of mass flux ratio in settling section: second section=1: 0.05～0.5.The average coke content of reactor settling section inner catalyst is 1～9%; The average coke content of reactor settling section inner catalyst is 2～6%.
Catalyzer in reactor settling section enters revivifier by pipeline to be generated after stripping, at breeding blanket inner catalyst, adopts the mixed gas of air or air and rare gas element to make charcoal.The catalyzer that catalyzer after regeneration and circulation line come enters reactor bottom, must make the catalyst carbon in reactor poor larger, carbon deposit is inhomogeneous, even if the average coke content of catalyzer reaches best coke content, can not make the selectivity of low-carbon alkene reach maximum.In addition, catalyst temperature after regeneration is higher, and the catalyst temperature that circulation line comes is lower, and the temperature of raw material is lower, it is even that three strands of larger materials of the temperature difference mix the temperature distributing disproportionation that must make in reactor in reactor, increased the difficulty that temperature of reactor is controlled.
Adopt method of the present invention, can be so that the degree that in revivifier, carbon deposited catalyst is made charcoal be easy to control by revivifier circulation line, the catalyst transport after regeneration is first mixed with a large amount of carbon deposited catalysts in settling vessel, then through circulation line, enters reactor.Adopt the method, no matter be that in revivifier, catalyzer adopts the mode of holomorphosis or the mode of incomplete regen-eration, with respect to regenerated catalyst in prior art, directly pass into reactor, can make the catalyst carbon deposit in reactor more even, thereby realize the object of controlling the best coke content of catalyst in reactor, can make selectivity of light olefin reach maximum value.In addition, catalyzer after regeneration first mixes and mixes with raw material with carbon deposition catalyst, makes to mix the interior temperature distribution of post-reactor more even, is easy to control.Therefore, method of the present invention can effectively improve the selectivity of low-carbon alkene in reaction process, and easy to operate, is easy to control.
Adopt technical scheme of the present invention: the oxygenatedchemicals in raw material is at least one in methyl alcohol or dme, described molecular sieve catalyst is SAPO type molecular sieve.The temperature of reactor is 350～600 ℃, and the pressure in reactor is counted 0～1MPa with gauge pressure, and raw material weight air speed is 0.1～20 hour
-1between.Temperature in revivifier is between 550～700 ℃, in revivifier, take gauge pressure pressure as 0～1MPa; Carbon deposition catalyst is in mass flux ratio first part in settling section: second section=1: 0.01～2; The average coke content of reactor settling section inner catalyst is 1～9%.The carbon base absorption rate of ethene+propylene reaches as high as 80.38% weight, has obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the invention.
In Fig. 1,1 is reactor settling section; 2 is reactor cycles pipeline; 3 is the feeding line of fluidized-bed reactor bottom; 4 is fluidized-bed reactor; 5 is regenerating medium entrance; 6 is riser regenerator; 7 is revivifier settling section; 8 is stripper; 9 is regeneration pipeline; 10 is revivifier circulation line; 11 is pipeline to be generated.
Raw material enters the fluidized-bed reactor 4 of reaction unit from the feeding line 3 of fluidized-bed reactor bottom, contact and react with the catalyzer of reactor cycles pipeline 2, gas-solid mixture enters the reactor settling section 1 of reaction unit after sharp separation, and gaseous products enters follow-up centrifugal station after cyclonic separator is deviate from catalyzer; Catalyzer first part catalyzer in reactor settling section enters fluidized-bed reactor 4 through reactor cycles pipeline 2, and second section enters riser regenerator 6 through pipeline 11 to be generated and the catalyzer merging of revivifier circulation line 10; Entering the carbon deposited catalyst of riser regenerator 6 and the regenerating medium of regenerating medium entrance 5 contacts after burning and enters revivifier settling section 7, the interior a part of catalyzer of revivifier settling section 7 enters stripper 8 strippings and delivers to reactor settling section 1 by regeneration pipeline 9, and a part of catalyzer enters riser regenerator 6 through revivifier circulation line 10 and the catalyzer merging of pipeline 11 to be generated.In revivifier, making charcoal of carbon deposited catalyst is easy to control, and can regulate the coke content of revivifier settling section inner catalyst by controlling revivifier circulation line.It is more even with the carbon deposit of carbon deposited catalyst mixing rear catalyst that regenerated catalyst enters reactor settling section, thereby can effectively improve the selectivity of low-carbon alkene.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1～3]
On reaction unit as shown in Figure 1, reactor adopts fast fluidized bed, temperature of reaction is 450 ℃, adopt respectively the feeding manner of methyl alcohol, dme, methyl alcohol+dme, raw material weight air speed is 5 hours-1, in gauge pressure reaction and regeneration pressure, be 0.01MPa, revivifier adopts riser tube, regenerating medium is air, regeneration temperature is 650 ℃, the thief hole of regenerator and spent agent lays respectively at regeneration pipeline 9 and pipeline to be generated 11, and on catalyzer, the analysis of carbon content adopts Infrared Carbon-sulphur high speed analysis instrument.The coke content of controlling reclaimable catalyst is 5.9% (weight percent), the coke content of regenerated catalyst is 05% (weight percent), it is first part that carbon deposition catalyst in settling section be take to mass flux ratio controls: second section=1: 0.1, make system run all right, control convenient.Catalyzer adopts the SAPO-34 modified catalyst of spray-dried moulding.Reactor outlet product adopts online gas chromatographic analysis, and experimental result is in Table 1.
Table 1
| Parameter | Type of feed | Methyl alcohol: dme (weight ratio) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 1 | Methyl alcohol | - | 43.14 | 34.25 | 77.39 |
| |
Dme | - | 43.49 | 33.78 | 77.27 |
| Embodiment 3 | Methyl alcohol+dme | 1∶1 | 43.85 | 33.81 | 77.66 |
[embodiment 4～6]
According to the condition described in embodiment 1, just change the type of catalyzer, experimental result is in Table 2.
Table 2
| Parameter | Catalyst type | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 4 | SAPO-11 | 8.52 | 23.12 | 31.64 |
| Embodiment 5 | SAPO-18 | 40.79 | 28.35 | 69.14 |
| Embodiment 6 | SAPO-56 | 28.66 | 22.69 | 51.35 |
[embodiment 7～10]
Condition according to described in embodiment 1, just changes temperature of reactor, and experimental result is in Table 3.
Table 3
| Parameter | Temperature of reactor, ℃ | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 7 | 350 | 25.29 | 26.57 | 51.86 |
| Embodiment 8 | 420 | 40.63 | 34.11 | 74.74 |
| Embodiment 9 | 500 | 48.26 | 32.12 | 80.38 |
| Embodiment 10 | 600 | 42.68 | 20.74 | 63.41 |
[embodiment 11～14]
Condition according to described in embodiment 1, just changes methyl alcohol weight space velocity, and experimental result is in Table 4.
Table 4
| Parameter | Methyl alcohol weight space velocity, hour -1 | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 11 | 0.15 | 41.97 | 31.48 | 73.45 |
| Embodiment 12 | 3.05 | 43.17 | 33.62 | 76.79 |
| Embodiment 13 | 8.16 | 43.85 | 33.65 | 77.50 |
| Embodiment 14 | 19.40 | 44.89 | 27.74 | 72.63 |
[embodiment 15～17]
Condition according to described in embodiment 1, just changes regenerator temperature, and experimental result is in Table 5.
Table 5
| Parameter | Regeneration temperature, ℃ | Regenerator coke content, % (weight) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 15 | 550 | 1.50 | 44.99 | 32.69 | 77.68 |
| Embodiment 16 | 600 | 1.15 | 44.07 | 33.58 | 77.65 |
| Embodiment 17 | 700 | 0.01 | 42.49 | 33.69 | 76.18 |
[embodiment 18～20]
According to the condition described in embodiment 1, reactor and revivifier adopt same press operation, change the pressure of reactor, revivifier, and experimental result is in Table 6.
Table 6
| Parameter | The pressure of reactor and revivifier, MPa | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 18 | 0.1 | 41.88 | 33.69 | 75.57 |
| Embodiment 19 | 0.3 | 39.78 | 32.86 | 73.64 |
| Embodiment 20 | 1 | 36.56 | 31.69 | 68.25 |
[embodiment 21～24]
According to the condition described in embodiment 1, just change the ratio of settling section two portions carbon deposition catalyst mass rate, experimental result is in Table 7.
Table 7
| Parameter | First part: second section (mass flux ratio) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 21 | 1∶0.02 | 20.33 | 10.01 | 30.34 |
| Embodiment 22 | 1∶0.05 | 44.54 | 30.20 | 74.74 |
| Embodiment 23 | 1∶0.5 | 40.44 | 35.37 | 75.81 |
| Embodiment 24 | 1∶2 | 40.30 | 35.04 | 75.34 |
[embodiment 25～28]
According to the condition described in embodiment 1, just change the coke content of reclaimable catalyst, experimental result is in Table 8.
Table 8
| Parameter | Spent agent coke content, % (weight) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Embodiment 25 | 1.00 | 39.04 | 35.48 | 74.52 |
| Embodiment 26 | 2.10 | 40.87 | 35.02 | 75.89 |
| Embodiment 27 | 7.60 | 40.36 | 30.14 | 70.50 |
| Embodiment 28 | 9.20 | 25.89 | 20.64 | 46.53 |
[comparative example 1～3]
Reaction unit is changed, and the catalyzer after regeneration is not transported to reactor settling section, but directly from reactor bottom, enters reactor, and all the other are all according to the condition described in embodiment 1,15,17, and experimental result is in Table 9.
Table 9
| Parameter | Regeneration temperature, ℃ | Regenerator coke content, % (weight) | Ethene carbon base absorption rate, % (weight) | Propylene carbon base absorption rate, % (weight) | Ethene+propylene carbon base absorption rate, % (weight) |
| Comparative example 1 | 650 | 0.50 | 42.44 | 33.91 | 76.35 |
| Comparative example 2 | 550 | 1.50 | 43.09 | 33.66 | 76.75 |
| Comparative example 3 | 700 | 0.01 | 41.63 | 33.69 | 75.32 |
Obviously, adopt method of the present invention, effectively improved oxygenatedchemicals and under molecular sieve catalyst exists, transformed the selectivity of producing light olefins, there is larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (1)
1. one kind is improved optionally method of converting oxygen-containing compound to low-carbon olefins, raw material enters the fluidized-bed reactor (4) of reaction unit from the feeding line (3) of fluidized-bed reactor bottom, the catalyzer coming with reactor cycles pipeline (2) contacts and reacts, gas-solid mixture enters the reactor settling section (1) of reaction unit after sharp separation, and gaseous products enters follow-up centrifugal station after cyclonic separator is deviate from catalyzer; Catalyzer first part catalyzer in reactor settling section enters fluidized-bed reactor (4) through reactor cycles pipeline (2), and the catalyzer merging that second section comes through pipeline to be generated (11) and revivifier circulation line (10) enters riser regenerator (6); The carbon deposited catalyst regenerating medium next with regenerating medium entrance (5) that enters riser regenerator (6) enters revivifier settling section (7) after contacting and burning, the interior a part of catalyzer of revivifier settling section (7) enters stripper (8) stripping and delivers to reactor settling section (1) by regeneration pipeline (9), and the catalyzer merging that a part of catalyzer comes through revivifier circulation line (10) and pipeline to be generated (11) enters riser regenerator (6);
Wherein, described fluidized-bed reactor adopts fast fluidized bed, and temperature of reaction is 500 ℃; Raw material is methyl alcohol, and raw material weight air speed is 5 hours
-1; In gauge pressure reaction and regeneration pressure, be 0.01MPa; Revivifier adopts riser tube, and regenerating medium is air, and regeneration temperature is 650 ℃; The thief hole of regenerator and spent agent lays respectively at regeneration pipeline (9) and pipeline to be generated (11), and on catalyzer, the analysis of carbon content adopts Infrared Carbon-sulphur high speed analysis instrument; It is 5.9% that the coke content of controlling reclaimable catalyst accounts for weight percent, and it is 0.5% that the coke content of regenerated catalyst accounts for weight percent, and it is first part that carbon deposition catalyst in settling section be take to mass flux ratio controls: second section=1: 0.1; Catalyzer adopts the SAPO-34 modified catalyst of spray-dried moulding; Reactor outlet product adopts online gas chromatographic analysis, and experimental result is: ethene carbon base absorption rate weight percentage 48.26%, propylene carbon base absorption rate weight percentage 32.12%, ethene+propylene carbon base absorption rate weight percentage 80.38%.
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| CN113385113A (en) * | 2020-03-13 | 2021-09-14 | 中国石油化工股份有限公司 | Method for improving yield of ethylene and propylene and fluidized bed reactor |
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