CN103372404A - Novel circulating fluidization device for preparing low-carbon olefin from methanol - Google Patents
Novel circulating fluidization device for preparing low-carbon olefin from methanol Download PDFInfo
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- CN103372404A CN103372404A CN2012101191149A CN201210119114A CN103372404A CN 103372404 A CN103372404 A CN 103372404A CN 2012101191149 A CN2012101191149 A CN 2012101191149A CN 201210119114 A CN201210119114 A CN 201210119114A CN 103372404 A CN103372404 A CN 103372404A
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Abstract
The invention relates to a novel circulating fluidization device for preparing low-carbon olefin from methanol. The device takes silicoaluminophosphate (SAPO-34) molecular sieve as a catalyst; a reactor adopts a fast fluidized bed to carry out catalytic reaction; a material return system of a regenerator can effectively control the circular flow rate of regenerated catalyst; two novel circulating fluidization reaction devices can be obtained according to the different heating ways of the regenerator. Compared with the prior art, the novel circulating fluidization device can reduce the loss of the catalyst, effectively controls the carbon deposition level of the catalyst, and improves the yield of the low-carbon olefin.
Description
Technical field
The present invention relates to a kind of ciculation fluidized device, especially relate to a kind of take methyl alcohol as the waste low-carbon alkene the ciculation fluidized reaction unit of (ethene, propylene).
Background technology
Preparing low carbon olefinic hydrocarbon with methanol technique is a kind of utilization by the methyl alcohol of natural gas or coal production is raw material, under the effect of zeolite or molecular sieve catalyst, produces the technology of the low-carbon alkenes such as ethene, propylene.Low-carbon alkene plays a part very important in modern petroleum and chemical industry industry as the basic organic chemical industry raw material.At present the method for preparing low-carbon olefins can be divided into two large classes generally: a class is the petroleum path that turns to representative with fluidized catalytic cracking, and another kind of is Non oil-based route take natural gas and coal as raw material.Because the China's oil reserves are relatively less and the continuous rise of oil price in recent years, development Non oil-based route preparing low-carbon olefins comes into one's own gradually.Wherein, preparing light olefins from methanol (Methane-to-Olefin, be called for short MTO) technique more and more is subject to attention both domestic and external as the non-oil new technology of tool potentiality.The MTO technology is to be improved on the basis of preparing gasoline by methanol (Methane-to-Gasoline the is called for short MTG) technology of announcement in 1984 by U.S. Mobil company to develop.This technique at first generates synthesis gas (CO and H take coal or natural gas as raw material
2), again synthesis gas is synthesized methyl alcohol, be low-carbon alkene with methanol conversion at last.
US4499327 is applied to MTO technology to the al silicate molecular sieve catalyst and has done detailed description, thinks that SAPO-34 is best suited for the catalyst of MTO technique.
U.S. associating oil product company discloses the fast fluidization MTO reaction unit that a kind of dense bed combines with fast bed in US6166282, conversion zone comprises the emulsion zone of bottom and two zones of transition region of top, methyl alcohol carries out the Partial Conversion reaction at emulsion zone, then promote the speed of grain flow by the undergauge transition region of top, take particle out of reaction zone, recycle after the sedimentation and regenerative operation.
The Dalian Chemistry and Physics Institute of the Chinese Academy of Sciences discloses a kind of ciculation fluidized reaction unit of dense bed with methyl alcohol or dimethyl ether preparing low-carbon olefins in CN1166478.This reaction unit is easy to derive reaction heat, and process is easy to control, and methyl alcohol and dimethyl ether treating capacity compare with the scale fixed bed reactors more than large ten times, the weight space velocity 1～10h of methyl alcohol or dimethyl ether
-1Lower, feed stock conversion is greater than 98%, and (yield of C2～C4) is greater than 90% for low-carbon alkene.
Tsing-Hua University discloses a kind of take dimethyl ether or methyl alcohol as raw material at CN1156416, utilize the gas-solid downstriker fluid bed super short contact time reactor that walks abreast.Enter the cyclic regeneration of regenerator reheating charcoal after catalyst is separated, reaction cycle is carried out.This anti-system has suppressed the generation of side reaction effectively by timely stopped reaction.The conversion ratio of dimethyl ether or methyl alcohol is greater than 98%, and yield of light olefins is greater than 93%.
Sinopec discloses the fast bed reaction unit that a kind of methyl alcohol or dimethyl ether are produced alkene in CN101333141.The reaction zone of this reaction unit is fast fluidized bed, and the lifting gas medium of standpipe is the above hydrocarbon of water vapour, methyl alcohol and C4, and the heat-obtaining mode of regenerator is the back-mixing formula.
Generally acknowledge in this area that catalyst can improve the yield of low-carbon alkene effectively in the MTO technique when reaching the carbon deposition quantity of certain level.And adjusting internal circulating load and recycle ratio are the control carbon deposition quantities, improve the most direct, the effective method of yield of light olefins.Prior art all exists carbon deposition quantity to distribute and is difficult to control, the defective that yield of light olefins is low.
Summary of the invention
Purpose of the present invention is exactly the New Cycle fluidizer that a kind of preparing light olefins from methanol is provided for the problem difficult, that carbon deposition quantity control is difficult, the catalyst circulation amount is little, yield of light olefins is low is amplified in the industry that overcomes above-mentioned prior art existence, the method has industry and amplifies simple, the catalyst circulation amount is easy to control, the advantage that yield of light olefins is high.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of New Cycle fluidizer of preparing light olefins from methanol comprises riser reactor, olefin recovery stripper, riser regenerator, waste gas degasser; The riser reactor bottom has carries device in advance, and outlet is connected in the stripper, and the exit is equipped with quick disconnector; Stripper mainly is comprised of stripping gas distributor and stripping baffles, and cyclone separator is equipped with on top, and two outlets are arranged at stripper bottom, an outlet through pipeline with carry in advance device and link to each other, another outlet links to each other bottom riser regenerator; Regenerator outlet links to each other with the waste gas degasser, and cyclone separator is equipped with in the outlet of degasser top, bottom the degasser through pipeline with carry in advance device and link to each other.
The New Cycle fluidizer of preparing light olefins from methanol can also comprise riser reactor, olefin recovery stripper, riser regenerator, secondary regenerator, waste gas degasser; The riser reactor bottom has carries device in advance, and outlet is connected in the stripper, and the exit is equipped with quick disconnector; Stripper mainly is comprised of stripping gas distributor and stripping baffles, and cyclone separator is equipped with on top, and two outlets are arranged at stripper bottom, an outlet through pipeline with carry in advance device and link to each other, another outlet links to each other bottom riser regenerator; Riser regenerator is connected to the secondary regenerator, and cyclone separator is equipped with on secondary regenerator top, and the bottom links to each other with degasser; The degasser top exit is equipped with cyclone separator, the bottom through pipeline with carry in advance device and link to each other.
This ciculation fluidized device use silicoaluminophosphamolecular molecular sieve catalyst or with the mixture of other catalyst, particle mean size 30～90 μ m.
Described riser reactor is upstriker fast bed reactor, raw material be methyl alcohol gas or with the mixture of carrier gas, 180～250 ℃ of inlet temperatures, 400～500 ℃ of reaction temperatures, weight space velocity 1～20h
-1, superficial gas velocity 0.7～3.0m/s, pressure 0～0.2MPa.
Described olefin recovery stripper is sloughed the low-carbon alkene that adheres in the catalyst, superficial gas velocity 0.003～0.020m/s.
The heat of catalyst regeneration is provided by fluidized gas or firing equipment, 500～700 ℃ of regeneration temperatures, recovery time 10～60min.
By the moving bed degasser regeneration off gases of adhering in the catalyst is sloughed superficial gas velocity 0.003～0.020m/s behind the catalyst regeneration.
Described secondary regenerator is moving-burden bed reactor, superficial gas velocity 0.005～0.200m/s.
Compared with prior art, the present invention has the following advantages:
(1) in the MTO technique catalyst when reaching the carbon deposition quantity of certain level, can effectively improve the yield of low-carbon alkene, the present invention is by the intensity of circulation of the catalyst of circulation and regeneration cycle in the adjusting catalyst, can effectively control the carbon deposition quantity of catalyst in rational level, thereby improve the yield of low-carbon alkene.
(2) the MTO reaction unit generally adopts the reactor that dense bed or dense bed combine with the conveying bed, the such device floor space is large, the control of catalyst carbon deposition horizontal distribution is very difficult, not only floor space is little for the lifting tubular type fast bed reactor that the present invention adopts, control relatively accurately the carbon distribution level, and the good gas-solid contact mode of fast bed and less back-mixing are so that the accessory substance in the final products is less.
(3) existing ciculation fluidized device, high such as fluid catalytic cracking (FCC) operating linear velocity, granules regeneration is frequent, not only catalyst abrasion is serious, and the high damage amount of running has very highland requirement to gas-solid separating device, the present invention has reduced operating linear velocity effectively by the endless form of two circulation lines, has reduced regeneration frequency, and then has avoided defects.
(4) revert system that generally adopts of existing ciculation fluidized reaction unit is for to have the control valve formula without feed bin, and pressure of silo is lower, operating flexibility is limited, the revert system that the aeration silo that the present invention adopts adds valve control type not only has very large operating flexibility, and control mode is various, can be fit to different technological requirements.
Description of drawings
Fig. 1 is structural representation of the present invention among the embodiment 1;
Fig. 2 is structural representation of the present invention among the embodiment 2.
Among the figure, 1a be material benzenemethanol gas or with the mixture of carrier gas, 2a is distributor, 3a is distribution grid, 4a is for carrying in advance device, 5a is riser reactor, 6a is quick disconnector, 7a is the olefin recovery stripper, 8a is stripping baffles, 9a is the stripping gas distributor, 10a is inner circulating tube, 11a is heat exchanger, 12a is valve, 13a is cyclone separator, 14a is gas products, 15a is the regeneration conveying gas, 16a is riser regenerator, 17a is the waste gas degasser, 18a is cyclone separator, 19a is flue gas, 20a is degassed gas, 21a is the regeneration cycle pipe, 22a is valve;
1b be material benzenemethanol gas or with the mixture of carrier gas, 2b is distributor, 3b is distribution grid, 4b is for carrying in advance device, 5b is riser reactor, 6b is quick disconnector, 7b is the olefin recovery stripper, 8b is stripping baffles, 9b is the stripping gas distributor, 10b is inner circulating tube, 11b is heat exchanger, 12b is valve, 13b is cyclone separator, 14b is gas products, 15b is conveying gas, 16b is riser regenerator, 17b is the secondary regenerator, 18b is flue gas, 19b is fluidized gas, 20b is degasser, 21b is degassed gas, 22b is cyclone separator, 23b is flue gas, 24b is the regeneration cycle pipe, 25b is valve.
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1
A kind of New Cycle fluidizer of preparing light olefins from methanol, its structure mainly comprise riser reactor 5a as shown in Figure 1, olefin recovery stripper 7a, riser regenerator 16a, waste gas degasser 17a; The bottom of riser reactor 5a is provided with and carries in advance device 4a, and outlet is connected among the olefin recovery stripper 7a, in the exit of riser reactor 5a quick disconnector 6a is installed; Olefin recovery stripper 7a mainly is comprised of stripping gas distributor 9a and stripping baffles 8a, cyclone separator 13a is equipped with on top in the olefin recovery stripper 7a, two outlets are arranged at olefin recovery stripper 7a bottom, one outlet with carry in advance device 4a and link to each other, another outlet links to each other bottom riser regenerator 16a; The outlet of riser regenerator 16a links to each other with waste gas degasser 17a, and cyclone separator 18a is equipped with in waste gas degasser 17a top outlet, the bottom of waste gas degasser 17a with carry in advance device 4a and link to each other.
When using this equipment, material benzenemethanol gas or enter by distributor 2a and distribution grid 3a with the mixture 1a of carrier gas is carried among the device 4a in advance, carry out catalytic reaction among the reactor 5a with entering after the catalyst mix from inner circulating tube 10a and regeneration cycle pipe 24a, generate the low-carbon alkene product.This ciculation fluidized device use silicoaluminophosphamolecular molecular sieve catalyst or with the mixture of other catalyst, particle mean size is the spheric catalyst of 30～90 μ m.Through the cyclone separator 13a of quick disconnector 6a and secondary, gas products separates with solid catalyst, and gas products 14a enters subsequent technique, and catalyst falls back to stripper 7a bottom.Stripping gas (water vapour or other gas) is entrained with device by stripping gas distributor 9a with the low-carbon alkene that adheres on the catalyst, and stripping baffles 8a can improve steam stripping efficiency.Clean catalyst is by outlet at bottom, and a part enters inner circulating tube 10a, is down to get back to after the reaction temperature by heat exchanger 11a and carries in advance the device bottom and continue to participate in reaction; Another part then enters among the riser regenerator 16a, be heated to regeneration temperature by regeneration conveying gas 15a or outside firing equipment, enter into degasser 17a after finishing regenerative response, flue gas 19a removes from cyclone separator 18a, by being blown into degassed gas 20a (water vapour, nitrogen or other gas) oxygen of catalyst surface and the hydrocarbon that produces of regenerating are blown off, the material-returning device that then is comprised of moving bed and valve 22a turns back to fresh catalyst by regeneration cycle pipe 21a proposes device participation reaction in advance.
Measure through particle speed, concentration meter, interior circulation and regeneration cycle flow rate were than 10: 1～200: 1; Riser reactor endoparticle intensity of circulation 20～300kg/ (m
2S), the particle time of staying 1～5s; Riser regenerator particle Residence Time 10～60min.
Embodiment 2
A kind of New Cycle fluidizer of preparing light olefins from methanol, its structure mainly comprise riser reactor 5b as shown in Figure 2, olefin recovery stripper 7b, secondary regenerator 17b, waste gas degasser 20b; The riser reactor bottom has carries device 4b in advance, and outlet is connected among the olefin recovery stripper 7b, and the exit is equipped with quick disconnector 6b; Stripper mainly is comprised of stripping gas distributor 9b and stripping baffles 8b, and cyclone separator 13b is equipped with on top, and two outlets are arranged at olefin recovery stripper 7b bottom, an outlet with carry in advance device 4b and link to each other, an outlet links to each other bottom regeneration riser 16b; Riser regenerator 16b is connected to regenerator 17b, and regenerator 17b is equipped with cyclone separator 18b in top, and the bottom links to each other with waste gas degasser 20b; Waste gas degasser 20b top exit is equipped with cyclone separator 22b, the bottom with carry in advance device 4b and link to each other.
Material benzenemethanol gas or enter by distributor 2b and distribution grid 3b with the mixture 1b of carrier gas is carried among the device 4b in advance, carries out catalytic reaction among the reactor 5b with entering after the catalyst mix from inner circulating tube 10b and regeneration cycle pipe 24b, generates the low-carbon alkene product.This ciculation fluidized device use silicoaluminophosphamolecular molecular sieve catalyst or with the mixture of other catalyst, particle mean size is the spheric catalyst of 30～90 μ m.Through the cyclone separator 13b of quick disconnector 6b and secondary, gas products separates with solid catalyst, and product 14b enters subsequent technique, and catalyst falls back to olefin recovery stripper 7b bottom.Stripping gas (water vapour or other gas) is entrained with device by distributor 9b with the low-carbon alkene that adheres on the catalyst, and stripping baffles 8b can improve steam stripping efficiency.Clean catalyst is by outlet at bottom, and a part enters inner circulating tube 10b, is down to get back to after the reaction temperature by heat exchanger 11b and carries in advance the device bottom and continue to participate in reaction; Another part then enters riser regenerator 16b bottom.Conveying gas 15b brings catalyst among the regenerator 17b into, be heated to regeneration temperature by fluidized gas 19b or external heat equipment, enter into degasser 20b after finishing regenerative response, flue gas 23b removes from cyclone separator 22b, by being blown into degassed gas 21b (water vapour, nitrogen or other gas) oxygen of catalyst surface and the hydrocarbon that produces of regenerating are blown off, the material-returning device that then is comprised of moving bed and valve 25b turns back to fresh catalyst by regeneration cycle pipe 24b proposes device participation reaction in advance.
Measure through particle speed, concentration meter, interior circulation and regeneration cycle flow rate were than 10: 1～200: 1; Riser reactor endoparticle intensity of circulation 20～300kg/ (m
2S), the particle time of staying 1～5s; Secondary regenerator particle Residence Time 30～60min.
Embodiment 3
The SAPO-34 catalyst of constant weight put into be the small fixed reactor, the aperture is equipped with less than the distribution grid of catalyst particle size in the bottom, is taken out of by gas to prevent catalyst.Pass into 200 ℃ methyl alcohol and nitrogen mixture (volume ratio 3: 1) from top, weight space velocity 2h
-1, 400 ℃ of reaction bed temperatures, normal pressure.Through gas chromatographic detection, methanol conversion＞99%, the yield 80% of ethene and propylene.
Embodiment 4
Measure the phosphorus content of the SAPO-34 catalyst after experiencing one period reaction time by DTG.According to the condition of embodiment 3, this catalyst is put into mini-reactor, inlet gas changes the gaseous mixture (volume ratio 7: 3) of 200 ℃ of methyl alcohol and water into, and product is detected online by gas-chromatography.Experimental result is: carbon deposition quantity (mass percent) 2%, methanol conversion＞99%, the yield 86% of ethene and propylene.
Embodiment 5
The SAPO-34 catalyst granules of the average grain diameter of packing in embodiment 1 shown device 65 μ m, reactor operating pressure 0.1MPa, 450 ℃ of operating temperatures.200 ℃, 100m
3The methyl alcohol of/h and superheated vapour mixture (volume ratio 7: 3) react weight space velocity 2h with catalyst mix
-1By valve control, getting back to the catalyst flow rate ratio of carrying in advance device and entering regenerator is 150: 1.Conveying gas uses the diesel oil of oxygen enrichment-air pre-mixing gas with catalyst combustion heating to 700 ℃, enters degasser after stopping 15min, finally turns back to premixed device and continues to participate in reaction.Experimental result is: carbon deposition quantity (mass percent) 1.7%, methanol conversion＞99%, ethene and propene yield 80%.
Embodiment 6
The SAPO-34 catalyst granules of the average grain diameter of packing in embodiment 2 shown devices 65 μ m, reactor operating pressure 0.2MPa, 450 ℃ of operating temperatures.200 ℃, 100m
3The methyl alcohol of/h and the mixture of aromatic hydrocarbon (volume ratio 12: 1) react weight space velocity 5h with catalyst mix
-1Valve control is arranged, and getting back to the catalyst flow rate ratio of carrying in advance device and entering regenerator is 50: 1.With air regenerated catalyst is transported in the fluid bed regenerator, uses built-in heat pipe that catalyst is heated to 600 ℃, enter degasser behind the stop 40min, turn back at last premixed device and participate in reaction.Experimental result is: carbon deposition quantity (mass percent) 0.4%, methanol conversion＞99%, ethene and propene yield 85%.
Comparative example 1
According to the condition of embodiment 5, the device spent material changes the SAPO-34 catalyst granules of 85 μ m into, and methyl alcohol and superheated vapour flow change 180m into
3/ h.Experimental result is: carbon deposition quantity 6.3%, methanol conversion＞99%, ethene and propene yield 82%.
Claims (8)
1. the New Cycle fluidizer of preparing light olefins from methanol, it is characterized in that, this device comprises riser reactor, the olefin recovery stripper, riser regenerator and waste gas degasser, the below import department of described riser reactor is provided with carries device in advance, the top outlet is arranged in the olefin recovery stripper, the exit, top is provided with quick disconnector, described olefin recovery stripper is comprised of stripping gas distributor and stripping baffles, cyclone separator is equipped with on top in the olefin recovery stripper, the bottom of olefin recovery stripper is provided with two outlets, one outlet with carry in advance device and be connected through pipeline, another outlet links to each other with the riser regenerator bottom, the outlet of described riser regenerator links to each other with the waste gas degasser, and described waste gas degasser top exports is equipped with cyclone separator, the bottom of waste gas degasser through pipeline with carry in advance device and be connected.
2. the New Cycle fluidizer of preparing light olefins from methanol according to claim 1 is characterized in that, is provided with the secondary regenerator between described riser regenerator and the waste gas degasser, and cyclone separator is equipped with on the top in the described secondary regenerator.
3. the New Cycle fluidizer of preparing light olefins from methanol according to claim 1 and 2, it is characterized in that, this ciculation fluidized device use silicoaluminophosphamolecular molecular sieve catalyst or with the mixture of other catalyst, particle mean size is the spheric catalyst of 30～90 μ m.
4. the New Cycle fluidizer of preparing light olefins from methanol according to claim 1 and 2 is characterized in that, described riser reactor is for promoting the tubular type fast bed.
5. the New Cycle fluidizer of preparing light olefins from methanol according to claim 1 and 2 is characterized in that, described olefin recovery stripper is taken the accompanying low-carbon alkene of particle out of.
6. the New Cycle fluidizer of preparing light olefins from methanol according to claim 1 and 2 is characterized in that, by the moving bed degasser regeneration off gases of adhering in the catalyst is sloughed behind the catalyst regeneration.
7. the New Cycle fluidizer of preparing light olefins from methanol according to claim 1 and 2 is characterized in that, the heat of catalyst regeneration is provided by fluidized gas or firing equipment.
8. the New Cycle fluidizer of preparing light olefins from methanol according to claim 2 is characterized in that, described secondary regenerator is moving-burden bed reactor.
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| CN105457567A (en) * | 2014-09-05 | 2016-04-06 | 中国石油化工股份有限公司 | Fluidized bed solid acid alkylation reaction and regeneration device and application method |
| CN109012513A (en) * | 2018-08-16 | 2018-12-18 | 中国石油大学(北京) | A kind of methanol to olefins reaction device |
| CN112110458A (en) * | 2020-09-11 | 2020-12-22 | 中国天辰工程有限公司 | Device and method for recycling waste heat and waste solids in reaction of preparing olefin from methanol |
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Cited By (4)
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| CN105457567A (en) * | 2014-09-05 | 2016-04-06 | 中国石油化工股份有限公司 | Fluidized bed solid acid alkylation reaction and regeneration device and application method |
| CN109012513A (en) * | 2018-08-16 | 2018-12-18 | 中国石油大学(北京) | A kind of methanol to olefins reaction device |
| CN109012513B (en) * | 2018-08-16 | 2020-11-03 | 中国石油大学(北京) | Methanol-to-olefin reactor |
| CN112110458A (en) * | 2020-09-11 | 2020-12-22 | 中国天辰工程有限公司 | Device and method for recycling waste heat and waste solids in reaction of preparing olefin from methanol |
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Application publication date: 20131030 |