CN102875289A - Method for preparing low-carbon olefins - Google Patents
Method for preparing low-carbon olefins Download PDFInfo
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- CN102875289A CN102875289A CN2011101934147A CN201110193414A CN102875289A CN 102875289 A CN102875289 A CN 102875289A CN 2011101934147 A CN2011101934147 A CN 2011101934147A CN 201110193414 A CN201110193414 A CN 201110193414A CN 102875289 A CN102875289 A CN 102875289A
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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 for preparing low-carbon alkene.
Technical background
Low-carbon alkene, namely 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 and the higher price of petroleum resources, 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 ethene processed, propylene.Wherein, the important alternative materials that is used for low-carbon alkene production 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, such as methyl alcohol, can be made by coal or Sweet natural gas, and technique is very ripe, can realize up to a million tonnes industrial scale.Because the popularity in 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 the US4499327 patent silicoaluminophosphamolecular molecular sieve catalyst is applied to preparing olefin by conversion of methanol technique and studies in great detail, think that SAPO-34 is the first-selected catalyzer of MTO technique.The 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 10 seconds degree, more even reach in the reaction time range of riser tube.
Technology and reactor that a kind of methanol conversion is low-carbon alkene have been announced among the US6166282, 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 greatly reduce.But there is the lower problem of yield of light olefins in the method.
The multiple riser reaction unit of having announced among the 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.Generally between 75～80%, there is the lower problem of yield of light olefins in the low-carbon alkene carbon base absorption rate equally in the method.
All there is the lower problem of yield of light olefins in prior art, and 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 that exists in the prior art, and a kind of new method for preparing low-carbon alkene is provided.The method is used 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 for preparing low-carbon alkene mainly may further comprise the steps: (1) first raw material enters the fluidized-bed reactor reaction zone, contacts with catalyzer, generation comprises the product of low-carbon alkene, forms simultaneously reclaimable catalyst; (2) a described reclaimable catalyst part enters revivifier regeneration, form regenerated catalyst, a part enters entrance end through the catalyst recirculation pipe and is positioned at described reaction zone outside, exit end is positioned at the riser tube of described reaction zone inside, contact with the second raw material, reclaimable catalyst is promoted in the described reaction zone, reclaimable catalyst enters from least one catalyst outlet that described riser tube in axial direction separates in the reaction zone of the first raw material feed distributing plate top, and the height that described riser tube is positioned at described reaction zone inside is at least 1/4 of described fluidized bed reaction zone height; (3) described regenerated catalyst returns fluidized-bed reactor reaction zone bottom; Wherein, described the first raw material comprises C 4 olefin, and the second raw material is mainly methyl alcohol.
In the technique scheme, described catalyzer is selected from SAPO-34; Described reclaimable catalyst enters from two catalyst outlets that described riser tube in axial direction separates in the reaction zone of the first raw material feed distributing plate top at least; Described reaction zone internal reaction condition is: temperature of reaction is 450～580 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 0.5～2.0 meter per second; Described reclaimable catalyst 50～80% returns reaction zone through riser tube, and 20～50% enter revivifier regeneration; The height that described riser tube is positioned at described reaction zone inside 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%; Described riser tube internal reaction condition is: temperature of reaction is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 4～8 meter per seconds.
Among the present invention, percentage of open area refers to the useful area of grid distributor, namely refers to the area summation in hole on the grid distributor face and the ratio of the grid distributor face total area.
The inventor is by the research discovery, and it is low-carbon alkene that the SAPO-34 molecular sieve catalyst both can transform methyl alcohol, can be low-carbon alkene at the conversion C 4 olefin of high conversion under the optimal conditions simultaneously.Adopt method of the present invention, enter the raw material that comprises C 4 olefin in fluidized-bed reactor reaction zone bottom, main high temperature with coming from revivifier, the 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 reaction zone inside, contact with reclaimable catalyst, because reclaimable catalyst contains a certain amount of coke content, has better Shape-selective, can be with the low-carbon alkene that is converted into of methyl alcohol highly selective, and unconverted methyl alcohol, the dme and some high-carbon hydrocarbon that generate out continue to react in fluidized bed reaction zone from riser tube afterwards, 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 fluidized-bed reactor reaction zone bottom with regenerated catalyst, regulate the average activity that C 4 olefin is converted into low-carbon alkene zone catalyzer, and the another one outlet enters fluidized bed reaction zone from the seedpod of the lotus shape gas-solid distribution apparatus at riser tube top, finally finishes the conversion of methyl alcohol.C 4 olefin of the present invention comes from methanol conversion and prepares isolated carbon four above hydrocarbon in the low-carbon alkene separation process.Therefore, by above means, can realize improving the purpose of yield of light olefins.
Adopt technical scheme of the present invention: described catalyzer is selected from SAPO-34; Described reclaimable catalyst enters from two catalyst outlets that described riser tube in axial direction separates in the reaction zone of the first raw material feed distributing plate top at least; Described reaction zone internal reaction condition is: temperature of reaction is 450～580 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 0.5～2.0 meter per second; Described reclaimable catalyst 50～80% returns reaction zone through riser tube, and 20～50% enter revivifier regeneration; The height that described riser tube is positioned at described reaction zone inside 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%, described riser tube internal reaction condition is: temperature of reaction is 400～500 ℃, reaction pressure is counted 0.01～0.3MPa with gauge pressure, the gas phase linear speed is 4～8 meter per seconds, the low-carbon alkene carbon base absorption rate reaches 89.17% (weight), low-carbon alkene carbon base absorption rate raising than prior art can reach 7%, has obtained preferably technique effect.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
Fig. 2 is the A-B sectional view among Fig. 1.
Among 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 the catalyst recirculation pipe; 7 is spent riser; 8 is gas-solid cyclone separator; 9 is the negative area; 10 is collection chamber; 11 is the product gas outlet pipeline; 12 is the second raw material charging; 13 are the 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 simultaneously reclaimable catalyst, 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 described reaction zone 2 outsides, exit end is positioned at the riser tube 7 of described reaction zone 2 inside, contact with the second raw material, reclaimable catalyst is promoted in the described reaction zone 2, reclaimable catalyst enters in the reaction zone 2 of the first raw material feed distributing plate 14 tops from least one catalyst outlet that described riser tube 7 in axial direction separates, and described regenerated catalyst returns fluidized-bed reactor reaction zone 2 bottoms.
The invention will be further elaborated below by embodiment, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
On reaction unit as shown in Figure 1, catalyzer adopts SAPO-34, the C 4 olefin massfraction is that 88% carbon four hydrocarbon mixtures enter the fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form simultaneously reclaimable catalyst, described reclaimable catalyst 50% enters revivifier regeneration, form regenerated catalyst, 50% enters entrance end through the catalyst recirculation pipe is positioned at the reaction zone outside, exit end is positioned at the riser tube of reaction zone inside, contact with methanol feedstock, reclaimable catalyst is promoted in the reaction zone, reclaimable catalyst enters from two catalyst outlets that riser tube in axial direction separates in the reaction zone of the first raw material feed distributing plate top, two catalyst outlets lay respectively at the riser tube top, the riser tube middle part, the riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, and percentage of open area is 0.5, and the height that riser tube is positioned at reaction zone inside is 1/3 of described fluidized bed reaction zone height.Reaction zone internal reaction condition is: temperature of reaction is 580 ℃, reaction pressure is counted 0.01MPa with gauge pressure, the gas phase linear speed is 2 meter per seconds, regenerated catalyst coke content massfraction is 0.02%, described riser tube internal reaction condition is: temperature of reaction is 500 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the 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 embodiment 1 described condition and step, the C 4 olefin massfraction is that 88% carbon four hydrocarbon mixtures enter the fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form simultaneously reclaimable catalyst, described reclaimable catalyst 20% enters revivifier regeneration, form regenerated catalyst, 80% enters entrance end through the catalyst recirculation pipe is positioned at the reaction zone outside, exit end is positioned at the riser tube of reaction zone inside, contact with methanol feedstock, reclaimable catalyst is promoted in the reaction zone, reclaimable catalyst enters from two catalyst outlets that riser tube in axial direction separates in the reaction zone of the first raw material feed distributing plate top, two catalyst outlets lay respectively at the riser tube top, the riser tube middle part, the riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, percentage of open area is 0.8, and the height that riser tube is positioned at reaction zone inside is 1/4 of described fluidized bed reaction zone height.Reaction zone internal reaction condition is: temperature of reaction is 450 ℃, reaction pressure is counted 0.01MPa with gauge pressure, the gas phase linear speed is 0.5 meter per second, regenerated catalyst coke content massfraction is 0.5%, described riser tube internal reaction condition is: temperature of reaction is 400 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the 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 embodiment 1 described condition and step, the C 4 olefin massfraction is that 88% carbon four hydrocarbon mixtures enter the fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form simultaneously reclaimable catalyst, described reclaimable catalyst 30% enters revivifier regeneration, form regenerated catalyst, 70% enters entrance end through the catalyst recirculation pipe is positioned at the reaction zone outside, exit end is positioned at the riser tube of reaction zone inside, contact with methanol feedstock, reclaimable catalyst is promoted in the reaction zone, reclaimable catalyst enters from two catalyst outlets that riser tube in axial direction separates in the reaction zone of the first raw material feed distributing plate top, two catalyst outlets lay respectively at the riser tube top, the riser tube middle part, the riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, percentage of open area is 0.8, and the height that riser tube is positioned at reaction zone inside is 1/2 of described fluidized bed reaction zone height.Reaction zone internal reaction condition is: temperature of reaction is 550 ℃, reaction pressure is counted 0.01MPa with gauge pressure, the gas phase linear speed is 0.8 meter per second, regenerated catalyst coke content massfraction is 0.12%, described riser tube internal reaction condition is: temperature of reaction is 470 ℃, and reaction pressure is counted 0.01MPa with gauge pressure, and the 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 embodiment 1 described condition and step, the C 4 olefin massfraction is that 94% carbon four hydrocarbon mixtures enter the fluidized-bed reactor reaction zone, contact with catalyzer, generation comprises the product of low-carbon alkene, form simultaneously reclaimable catalyst, described reclaimable catalyst 30% enters revivifier regeneration, form regenerated catalyst, 70% enters entrance end through the catalyst recirculation pipe is positioned at the reaction zone outside, exit end is positioned at the riser tube of reaction zone inside, contact with methanol feedstock, reclaimable catalyst is promoted in the reaction zone, reclaimable catalyst enters from the catalyst outlet of riser tube top in the reaction zone of the first raw material feed distributing plate top, the riser tube top exit arranges seedpod of the lotus shape gas-solid distribution apparatus, and percentage of open area is 0.8, and the height that riser tube is positioned at reaction zone inside is 2/3 of described fluidized bed reaction zone height.Reaction zone internal reaction condition is: temperature of reaction is 570 ℃, reaction pressure is counted 0.3MPa with gauge pressure, the gas phase linear speed is 0.6 meter per second, regenerated catalyst coke content massfraction is 0.15%, described riser tube internal reaction condition is: temperature of reaction is 480 ℃, and reaction pressure is counted 0.3MPa with gauge pressure, and the 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]
According to embodiment 1 described condition and step, riser tube is not set, methyl alcohol and C 4 olefin diameter enter reaction zone from fluidized-bed reactor reaction zone bottom, 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 purpose that improves yield of light olefins, have larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (9)
1. method for preparing low-carbon alkene mainly may further comprise the steps:
(1) first raw material enters the fluidized-bed reactor reaction zone, contacts with catalyzer, generates the product that comprises low-carbon alkene, forms simultaneously reclaimable catalyst;
(2) a described reclaimable catalyst part enters revivifier regeneration, form regenerated catalyst, a part enters entrance end through the catalyst recirculation pipe and is positioned at described reaction zone outside, exit end is positioned at the riser tube of described reaction zone inside, contact with the second raw material, reclaimable catalyst is promoted in the described reaction zone, reclaimable catalyst enters from least one catalyst outlet that described riser tube in axial direction separates in the reaction zone of the first raw material feed distributing plate top, and the height that described riser tube is positioned at described reaction zone inside is at least 1/4 of described fluidized bed reaction zone height;
(3) described regenerated catalyst returns fluidized-bed reactor reaction zone bottom;
Wherein, described the first raw material comprises C 4 olefin, and the second raw material is mainly methyl alcohol.
2. the described method for preparing low-carbon alkene according to claim 1 is characterized in that described catalyzer is selected from SAPO-34.
3. the described method for preparing low-carbon alkene according to claim 1 is characterized in that described reclaimable catalyst enters in the reaction zone of the first raw material feed distributing plate top at least from two catalyst outlets that described riser tube in axial direction separates.
4. the described method for preparing low-carbon alkene according to claim 1, it is characterized in that described reaction zone internal reaction condition is: temperature of reaction is 450～580 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 0.5～2.0 meter per second.
5. the described method for preparing low-carbon alkene according to claim 1 is characterized in that described reclaimable catalyst 50～80% returns reaction zone through riser tube, and 20～50% enter revivifier regeneration.
6. the described method for preparing low-carbon alkene according to claim 1 is characterized in that the height that described riser tube is positioned at described reaction zone inside is at least 1/3 of described fluidized bed reaction zone height.
7. the described method for preparing low-carbon alkene according to claim 1 is characterized in that 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.
8. the described method for preparing low-carbon alkene according to claim 1 is characterized in that described regenerated catalyst coke content massfraction is 0.02～0.5%.
9. the described method for preparing low-carbon alkene according to claim 1, it is characterized in that described riser tube internal reaction condition is: temperature of reaction is 400～500 ℃, and reaction pressure is counted 0.01～0.3MPa with gauge pressure, and the gas phase linear speed is 4～8 meter per seconds.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015081489A1 (en) | 2013-12-03 | 2015-06-11 | 中国科学院大连化学物理研究所 | Method for preparing a light olefin using an oxygen-containing compound |
| WO2015081494A1 (en) | 2013-12-03 | 2015-06-11 | 中国科学院大连化学物理研究所 | Reaction device for preparing light olefins from methanol and/or dimethyl ether |
| WO2015081484A1 (en) | 2013-12-03 | 2015-06-11 | 中国科学院大连化学物理研究所 | Method for preparing a light olefin using an oxygen-containing compound, and device for use thereof |
| 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 |
| CN114377621A (en) * | 2020-10-16 | 2022-04-22 | 中国科学院大连化学物理研究所 | Fluidized bed reactor, device and application |
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| 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 |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015081489A1 (en) | 2013-12-03 | 2015-06-11 | 中国科学院大连化学物理研究所 | Method for preparing a light olefin using an oxygen-containing compound |
| WO2015081494A1 (en) | 2013-12-03 | 2015-06-11 | 中国科学院大连化学物理研究所 | Reaction device for preparing light olefins from methanol and/or dimethyl ether |
| WO2015081484A1 (en) | 2013-12-03 | 2015-06-11 | 中国科学院大连化学物理研究所 | Method for preparing a light olefin using an oxygen-containing compound, and device for use thereof |
| US9725375B2 (en) | 2013-12-03 | 2017-08-08 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Method for preparing a light olefin with an oxygen-containing compound |
| US9827544B2 (en) | 2013-12-03 | 2017-11-28 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Reaction device for preparing light olefins from methanol and/or dimethyl ether |
| 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 |
| CN114377621A (en) * | 2020-10-16 | 2022-04-22 | 中国科学院大连化学物理研究所 | Fluidized bed reactor, device and application |
| 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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