CN102875289B - Method for preparing low-carbon olefins - Google Patents
Method for preparing low-carbon olefins Download PDFInfo
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- CN102875289B CN102875289B CN201110193414.7A CN201110193414A CN102875289B CN 102875289 B CN102875289 B CN 102875289B CN 201110193414 A CN201110193414 A CN 201110193414A CN 102875289 B CN102875289 B CN 102875289B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/584—Recycling of catalysts
Abstract
The invention relates to a method for preparing low-carbon olefins, mainly solving the problem of low yield of low-carbon olefins in the prior art. The method disclosed herein mainly comprises the following steps: (1) letting a first raw material enter into a fluidized bed reaction zone to contact with a catalyst to generate a product containing low-carbon olefins and simultaneously form a spent catalyst; (2) letting a part of the spent catalyst enter into a regenerator for regenerating to form a regenerated catalyst, letting other part of the spent catalyst enter into a riser to contact with a second raw material to rise the spent catalyst into the reaction zone, wherein the outlet end of the riser is arranged in the reaction zone, and the height of the part of the riser in the reaction zone is at least 1/4 the height of the fluidized bed reaction zone; and (3) letting the regenerated catalyst return to the fluidized bed reaction zone, wherein the first raw material contains C4 hydrocarbons, the second raw material mainly contains methanol. The method disclosed herein disclosed herein well solves the problem and can be used in the industrial production of low-carbon olefins.
Description
Technical field
The present invention relates to a kind of method of preparing low-carbon alkene.
Technical background
Low-carbon alkene, ethene and propylene, be 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 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 the technology that alternative materials transforms ethene processed, propylene.Wherein, the important alternative materials of producing for low-carbon alkene of one class is oxygenatedchemicals, such as 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 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.
Technology and reactor that a kind of methanol conversion is low-carbon alkene in US6166282, have been announced, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu of gas speed has reacted, rise to after the fast subregion that internal diameter diminishes rapidly, adopt special gas-solid separation equipment initial gross separation to go out most entrained catalyst.Due to reaction after product gas and catalyzer sharp separation, 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 greatly reduce.But there is the problem that yield of light olefins is lower in the method.
The multiple riser reaction unit of having announced in CN1723262 with central catalyst return is low-carbon alkene technique 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 gas product are separated.In the method generally between 75～80%, there is the problem that yield of light olefins is lower in low-carbon alkene carbon base absorption rate equally.
All there is the problem that yield of light olefins is lower 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 lower problem of yield of light olefins existing in prior art, and a kind of new method of preparing low-carbon alkene is provided.The method, for the production of low-carbon alkene, has advantages of that yield of light olefins is higher.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of method of preparing low-carbon alkene, mainly comprises the following steps: (1) first raw material enters fluidized-bed reactor reaction zone, contacts with catalyzer, generation comprises the product of low-carbon alkene, forms reclaimable catalyst simultaneously, (2) a described reclaimable catalyst part enters revivifier regeneration, form regenerated catalyst, a part enters entrance end through catalyst recirculation pipe and is positioned at outside, described reaction zone, exit end is positioned at the riser tube of inside, described reaction zone, contact with the second raw material, reclaimable catalyst is promoted in described reaction zone, in at least one catalyst outlet that reclaimable catalyst in axial direction separates from described riser tube, enter in the reaction zone of the first raw material feed distributing plate top, the height that described riser tube is positioned at inside, described reaction zone is at least 1/4 of described fluidized bed reaction zone height, (3) described regenerated catalyst returns to bottom, fluidized-bed reactor reaction zone, wherein, described the first raw material comprises C 4 olefin, and the second raw material is mainly methyl alcohol.
In technique scheme, described catalyzer is selected from SAPO-34; In at least two catalyst outlets that described reclaimable catalyst in axial direction separates from described riser tube, enter in the reaction zone of the first raw material feed distributing plate top; In described reaction zone, reaction conditions is: temperature of reaction is 450～580 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and gas phase linear speed is 0.5～2.0 meter per second; Described reclaimable catalyst 50～80% returns to reaction zone through riser tube, and 20～50% enter revivifier regeneration; The height that described riser tube is positioned at inside, described reaction zone is at least 1/3 of described fluidized bed reaction zone height; Described riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, and percentage of open area is 0.5～0.8; Described regenerated catalyst coke content massfraction is 0.02～0.5%; In described riser tube, reaction conditions is: temperature of reaction is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and gas phase linear speed is 4～8 meter per seconds.
In the present invention, percentage of open area refers to the useful area of grid distributor, namely refers to the area summation in hole on grid distributor face and the ratio of the grid distributor face total area.
The inventor finds by research, and it is low-carbon alkene that SAPO-34 molecular sieve catalyst both can transform methyl alcohol, can at the conversion C 4 olefin of high conversion under optimal conditions, be low-carbon alkene simultaneously.Adopt method of the present invention, in bottom, fluidized-bed reactor reaction zone, enter the raw material that comprises C 4 olefin, the main high temperature with coming from revivifier, high activated catalyst contact, under lower linear speed, the generation low-carbon alkene of high conversion, and methyl alcohol enters in the riser tube that gos deep into inside, reaction zone, contact with reclaimable catalyst, because reclaimable catalyst contains a certain amount of coke content, there is preferably Shape-selective, can be by the low-carbon alkene that is converted into of methyl alcohol highly selective, and unconverted methyl alcohol, the dme generating and some high-carbon hydrocarbon continue to react in fluidized bed reaction zone out from riser tube, thereby guarantee higher methyl alcohol total conversion rate.Riser tube arranges at least one catalyst outlet, preferred embodiment is that at least two catalyst outlets are set, one of them mixes in bottom, fluidized-bed reactor reaction zone with regenerated catalyst, regulate C 4 olefin to be converted into the average activity of low-carbon alkene region catalyzer, and another one outlet enters fluidized bed reaction zone from the seedpod of the lotus shape gas-solid distribution apparatus at riser tube top, finally complete the conversion of methyl alcohol.C 4 olefin of the present invention comes from methanol conversion and prepares the above hydrocarbon of isolated carbon four in low-carbon alkene separation process.Therefore,, by above means, can realize the object that improves yield of light olefins.
Adopt technical scheme of the present invention: described catalyzer is selected from SAPO-34; In at least two catalyst outlets that described reclaimable catalyst in axial direction separates from described riser tube, enter in the reaction zone of the first raw material feed distributing plate top; In described reaction zone, reaction conditions is: temperature of reaction is 450～580 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and gas phase linear speed is 0.5～2.0 meter per second; Described reclaimable catalyst 50～80% returns to reaction zone through riser tube, and 20～50% enter revivifier regeneration; The height that described riser tube is positioned at inside, described reaction zone is at least 1/3 of described fluidized bed reaction zone height; Described riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, and percentage of open area is 0.5～0.8; Described regenerated catalyst coke content massfraction is 0.02～0.5%, in described riser tube, reaction conditions is: temperature of reaction is 400～500 ℃, reaction pressure is counted 0.01～0.3MPa with gauge pressure, gas phase linear speed is 4～8 meter per seconds, low-carbon alkene carbon base absorption rate reaches 89.17% (weight), than the low-carbon alkene carbon base absorption rate of prior art, improve and can reach 7%, obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the invention.
Fig. 2 is the A-B sectional view in Fig. 1.
In Fig. 1,1 is the first material feeding tube line; 2 is fluidized bed reaction zone; 3 is gas-solid separation equipment; 4 is inclined tube to be generated; 5 is regenerator sloped tube; 6 is catalyst recirculation pipe; 7 is spent riser; 8 is gas-solid cyclone separator; 9 is negative area; 10 is collection chamber; 11 is product gas outlet pipeline; 12 is the second raw material charging; 13 is reclaimable catalyst outlet; 14 is the first raw material feed distributing plate.
The first raw material enters fluidized-bed reactor reaction zone 2, contact with catalyzer, generation comprises the product of low-carbon alkene, form reclaimable catalyst simultaneously, a described reclaimable catalyst part enters revivifier regeneration, form regenerated catalyst, a part enters entrance end through catalyst recirculation pipe 6 and is positioned at 2 outsides, described reaction zone, exit end is positioned at the riser tube 7 of 2 inside, described reaction zone, contact with the second raw material, reclaimable catalyst is promoted in described reaction zone 2, in at least one catalyst outlet that reclaimable catalyst in axial direction separates from described riser tube 7, enter in the reaction zone 2 of the first raw material feed distributing plate 14 tops, described regenerated catalyst returns to 2 bottoms, fluidized-bed reactor reaction zone.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
On reaction unit as shown in Figure 1, catalyzer adopts SAPO-34, C 4 olefin massfraction is that 88% carbon four hydrocarbon mixtures enter fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form reclaimable catalyst simultaneously, described reclaimable catalyst 50% enters revivifier regeneration, form regenerated catalyst, 50% enters entrance end through catalyst recirculation pipe is positioned at outside, reaction zone, exit end is positioned at the riser tube of inside, reaction zone, contact with methanol feedstock, reclaimable catalyst is promoted in reaction zone, in two catalyst outlets that reclaimable catalyst in axial direction separates from riser tube, enter in the reaction zone of the first raw material feed distributing plate top, two catalyst outlets lay respectively at riser tube top, riser tube middle part, riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, percentage of open area is 0.5, the height that riser tube is positioned at inside, reaction zone is 1/3 of described fluidized bed reaction zone height.In reaction zone, reaction conditions is: temperature of reaction is 580 ℃, reaction pressure is counted 0.01MPa with gauge pressure, gas phase linear speed is 2 meter per seconds, regenerated catalyst coke content massfraction is 0.02%, in described riser tube, reaction conditions is: temperature of reaction is 500 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and gas phase linear speed is 8 meter per seconds, reactor product adopts gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate of reactor outlet is 89.17% (weight).
[embodiment 2]
According to condition and the step described in embodiment 1, C 4 olefin massfraction is that 88% carbon four hydrocarbon mixtures enter fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form reclaimable catalyst simultaneously, described reclaimable catalyst 20% enters revivifier regeneration, form regenerated catalyst, 80% enters entrance end through catalyst recirculation pipe is positioned at outside, reaction zone, exit end is positioned at the riser tube of inside, reaction zone, contact with methanol feedstock, reclaimable catalyst is promoted in reaction zone, in two catalyst outlets that reclaimable catalyst in axial direction separates from riser tube, enter in the reaction zone of the first raw material feed distributing plate top, two catalyst outlets lay respectively at riser tube top, riser tube middle part, riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, percentage of open area is 0.8, the height that riser tube is positioned at inside, reaction zone is 1/4 of described fluidized bed reaction zone height.In reaction zone, reaction conditions is: temperature of reaction is 450 ℃, reaction pressure is counted 0.01MPa with gauge pressure, gas phase linear speed is 0.5 meter per second, regenerated catalyst coke content massfraction is 0.5%, in described riser tube, reaction conditions is: temperature of reaction is 400 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and gas phase linear speed is 4 meter per seconds, reactor product adopts gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate of reactor outlet is 85.27% (weight).
[embodiment 3]
According to condition and the step described in embodiment 1, C 4 olefin massfraction is that 88% carbon four hydrocarbon mixtures enter fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form reclaimable catalyst simultaneously, described reclaimable catalyst 30% enters revivifier regeneration, form regenerated catalyst, 70% enters entrance end through catalyst recirculation pipe is positioned at outside, reaction zone, exit end is positioned at the riser tube of inside, reaction zone, contact with methanol feedstock, reclaimable catalyst is promoted in reaction zone, in two catalyst outlets that reclaimable catalyst in axial direction separates from riser tube, enter in the reaction zone of the first raw material feed distributing plate top, two catalyst outlets lay respectively at riser tube top, riser tube middle part, riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, percentage of open area is 0.8, the height that riser tube is positioned at inside, reaction zone is 1/2 of described fluidized bed reaction zone height.In reaction zone, reaction conditions is: temperature of reaction is 550 ℃, reaction pressure is counted 0.01MPa with gauge pressure, gas phase linear speed is 0.8 meter per second, regenerated catalyst coke content massfraction is 0.12%, in described riser tube, reaction conditions is: temperature of reaction is 470 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and gas phase linear speed is 5 meter per seconds, reactor product adopts gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate of reactor outlet is 87.09% (weight).
[embodiment 4]
According to condition and the step described in embodiment 1, C 4 olefin massfraction is that 94% carbon four hydrocarbon mixtures enter fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form reclaimable catalyst simultaneously, described reclaimable catalyst 30% enters revivifier regeneration, form regenerated catalyst, 70% enters entrance end through catalyst recirculation pipe is positioned at outside, reaction zone, exit end is positioned at the riser tube of inside, reaction zone, contact with methanol feedstock, reclaimable catalyst is promoted in reaction zone, reclaimable catalyst enters in the reaction zone of the first raw material feed distributing plate top from the catalyst outlet of riser tube top, riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, percentage of open area is 0.8, the height that riser tube is positioned at inside, reaction zone is 2/3 of described fluidized bed reaction zone height.In reaction zone, reaction conditions is: temperature of reaction is 570 ℃, reaction pressure is counted 0.3MPa with gauge pressure, gas phase linear speed is 0.6 meter per second, regenerated catalyst coke content massfraction is 0.15%, in described riser tube, reaction conditions is: temperature of reaction is 480 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and gas phase linear speed is 4.5 meter per seconds, reactor product adopts gas chromatographic analysis, and the low-carbon alkene carbon base absorption rate of reactor outlet is 86.13% (weight).
[comparative example 1]
Condition and step according to described in embodiment 1, do not arrange riser tube, and methyl alcohol and C 4 olefin diameter enter reaction zone from bottom, fluidized-bed reactor reaction zone, and the low-carbon alkene carbon base absorption rate of reactor outlet is 82.15% (weight).
Obviously, adopt method of the present invention, can reach the object that improves yield of light olefins, there is larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (9)
1. a method of preparing low-carbon alkene, mainly comprises the following steps:
(1) first raw material enters fluidized-bed reactor reaction zone, contacts with catalyzer, generates the product that comprises low-carbon alkene, forms reclaimable catalyst simultaneously;
(2) a described reclaimable catalyst part enters revivifier regeneration, form regenerated catalyst, a part enters entrance end through catalyst recirculation pipe and is positioned at outside, described reaction zone, exit end is positioned at the riser tube of inside, described reaction zone, contact with the second raw material, reclaimable catalyst is promoted in described reaction zone, in at least one catalyst outlet that reclaimable catalyst in axial direction separates from described riser tube, enter in the reaction zone of the first raw material feed distributing plate top, the height that described riser tube is positioned at inside, described reaction zone is at least 1/4 of described fluidized bed reaction zone height,
(3) described regenerated catalyst returns to bottom, fluidized-bed reactor reaction zone;
Wherein, described the first raw material comprises C 4 olefin, and the second raw material is mainly methyl alcohol.
2. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that described catalyzer is selected from SAPO-34.
3. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that entering in the reaction zone of the first raw material feed distributing plate top at least two catalyst outlets that described reclaimable catalyst in axial direction separates from described riser tube.
4. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that in described reaction zone, reaction conditions is: temperature of reaction is 450～580 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, gas phase linear speed is 0.5～2.0 meter per second.
5. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that described reclaimable catalyst 50～80% returns to reaction zone through riser tube, 20～50% enter revivifier regeneration.
6. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that the height that described riser tube is positioned at inside, described reaction zone is at least 1/3 of described fluidized bed reaction zone height.
7. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that described riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, percentage of open area is 0.5～0.8.
8. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that described regenerated catalyst coke content massfraction is 0.02～0.5%.
9. prepare according to claim 1 the method for low-carbon alkene, it is characterized in that in described riser tube, reaction conditions is: temperature of reaction is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and gas phase linear speed is 4～8 meter per seconds.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9718743B2 (en) | 2013-12-03 | 2017-08-01 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Method for preparing a light olefin using an oxygen-containing compound, and device for use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101763864B1 (en) | 2013-12-03 | 2017-08-01 | 달리안 인스티튜트 오브 케미컬 피직스, 차이니즈 아카데미 오브 사이언시즈 | Reaction device for preparing light olefins from methanol and/or dimethyl ether |
| SG11201604429VA (en) | 2013-12-03 | 2016-07-28 | Dalian Chemical Physics Inst | Method for preparing a light olefin using an oxygen-containing compound |
| CN105695614A (en) * | 2016-04-20 | 2016-06-22 | 郑州大学 | Method for identifying polymorphism of human breast cancer genes BRCA1 rs8176318 by aid of NsiI |
| CN114377621B (en) * | 2020-10-16 | 2024-03-19 | 中国科学院大连化学物理研究所 | Fluidized bed reactor, device and application |
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| US6166282A (en) * | 1999-08-20 | 2000-12-26 | Uop Llc | Fast-fluidized bed reactor for MTO process |
| CN101164684A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Combined fluidized bed reactor |
| CN101165026A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from methanol and dimethyl ether |
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| US6166282A (en) * | 1999-08-20 | 2000-12-26 | Uop Llc | Fast-fluidized bed reactor for MTO process |
| CN101164684A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Combined fluidized bed reactor |
| CN101165026A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from methanol and dimethyl ether |
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| US9718743B2 (en) | 2013-12-03 | 2017-08-01 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Method for preparing a light olefin using an oxygen-containing compound, and device for use thereof |
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