CN104248940A - Multistage radial stationary bed reaction system and method for producing propylene from oxy-compound as raw material - Google Patents
Multistage radial stationary bed reaction system and method for producing propylene from oxy-compound as raw material Download PDFInfo
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- CN104248940A CN104248940A CN201410492519.6A CN201410492519A CN104248940A CN 104248940 A CN104248940 A CN 104248940A CN 201410492519 A CN201410492519 A CN 201410492519A CN 104248940 A CN104248940 A CN 104248940A
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Abstract
The invention discloses a multistage radial stationary bed reaction system and a method for producing propylene from an oxy-compound as a raw material. The radial stationary bed reaction system comprises a plurality of radial stationary bed reactors and interstage mixers, wherein the radial stationary bed reactors are barrel-shaped reactors; a reaction gas inlet, a reaction gas pre-distributor, a product gas outlet, a catalyst inlet and a catalyst outlet are arranged at the upper part and the lower part of each barrel-shaped reactor respectively; a porous wall inner barrel and a porous wall outer barrel which are coaxial with a cylindrical housing are arranged in the barrel-shaped reactor; a catalyst filling region is arranged between each porous wall inner barrel and each porous wall outer barrel; a catalyst upper seal plate and a lower seal plate are arranged at the upper part and the lower part of each catalyst filling region respectively. The multistage radial stationary bed reaction system can be used for assisting in interstage quenching of raw material gas and circulation of part of products by the tandem radial stationary bed reactors, and the problems of non-uniform fluid distribution, jet nozzle blockage, low propylene yield and the like of a conventional radial reactor can be remarkably improved.
Description
Technical field
The present invention relates to a kind of production system and method for propylene, particularly relating to a kind of for taking oxygenatedchemicals as multistage radial fixed-bed reaction system and the method thereof that propylene produced by raw material.
Background technology
Propylene is a kind of important basic chemical industry raw material in modern chemical industry, its total amount 95% from naphtha steam cracking coproduction and fluid catalytic cracking (FCC) by-product.By global crude oil price continuous rise, and ethylene raw is to the impact of the lighter hydrocarbons transfer tendencies such as ethane, the sustainable growth of global propylene demand gap.Meanwhile, preparing propylene from methanol (MTP) technique of producing propylene with coal-based methanol or natural gas/shale gas base methyl alcohol for raw material is subject to various countries' favor day by day.For the energy resource structure of China's " rich coal, oil starvation, weak breath ", develop, with coal-based methanol or MTP technique that natural gas/shale gas base methyl alcohol is raw material, there is the higher market competitiveness and far-reaching strategic importance.
UOP/Hydro company adopts SAPO-34 molecular sieve as catalyst and coordinates fluidized-bed reactor to have developed methanol-to-olefins (MTO) technique.Because fluid bed inside is tending towards complete mixing flow, bed temperature distribution uniform and be easy to control.But because catalyst granules is less, carry phenomenon secretly seriously, larger on the impact of later separation workshop section.Lu Qi (Lurgi) company have developed the industrialized MTP preparing propylene from methanol device of world head cover, and this device adopts 4 fixed bed reactors.First methyl alcohol be partially converted into dimethyl ether in 1 dimethyl ether reactor (DME reactor), the mixture of methyl alcohol, dimethyl ether and water and process steam subsequently, C2 and the C4 ~ C6 hydro carbons of circulation is mixed into MTP reactor and produces propylene, MTP reactor has 3, normal adopts when running 2 to open 1 standby mode to operate.
At present, existing multinomial patented technology relates to this field of MTP reactor both at home and abroad.Chinese patent CN 201220212924.4 discloses a kind of axially successively increment type cold shock formula preparing propylene from methanol fixed bed reactors.Arrange 4 ~ 6 beds in this reactor, thickness of bed layer increases progressively vertically gradually.Be provided with 10 ~ 20 unstripped gas and material liquid nozzle between bed and bed, by the mode of unstripped gas cold shock, the reacting gas flowing out a upper bed lowered the temperature and supplemented methyl alcohol, dimethyl ether raw material.Due to MTP reaction be adapted at low methanol partial pressure under carry out, therefore in order to control reactor bed pressure drop, the thickness of this catalyst in reactor bed is between 250mm ~ 700mm, if inevitable reactor diameter can be very large when methyl alcohol treating capacity is very large, and the nozzle quantity of quench gas is limited above each bed, the uneven appearance causing uniform focus of local mixing therefore may be caused, and along with the accumulation of service time, nozzle also may block, and affects the even running of reactor.International monopoly WO 2004018089 also discloses a kind of similar multistage thin-film fixed bed reactor, although such reactor separate unit treating capacity is large, efficiency is higher, but still can not overcome the problem of above-mentioned raw materials distribution inequality and spray nozzle clogging.
Chinese patent ZL 200810120839.3 discloses a kind of MTP radially moving bed reactor.Adopt moving-burden bed reactor to carry out MTP reaction the operation cycle of the medium deactivation rate of ZSM-5 catalyst and moving-burden bed reactor to be matched, make catalyst remain at best reactivity worth.Meanwhile, because MTP reaction is a strong exothermal reaction, this patent is also provided with cooling zone in moving bed inside, adopts the mode of logical cooling medium to shift out reaction heat, prevents the too high generation temperature runaway of bed temperature.But because the internal structure of moving bed own is just comparatively complicated, more built-in cooling device more can increase the complexity of device internal structure, all may affect to the processing of reactor and running.
Make a general survey of existing MTP axial restraint bed bioreactor or radially moving bed reactor, the problem that there is internal structure complexity all more or less, no matter be the setting of nozzle or the interpolation of internal exchanger, all can increase the complexity of structure of reactor, increase manufacturing cost.Meanwhile, also all more or less there is certain defect, the problem of the feed distribution inequality that the common charging of such as liquid phase may bring in the combining form and feeding manner etc. of its reactor.
Summary of the invention
Technical problem solved by the invention is the reactor inner fluid skewness existed in conventional art, and inside reactor complex structure and reaction process arrange the problems such as unreasonable.For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of radial fixed-bed reaction system of the multistage radial fixed-bed reaction system for taking oxygenatedchemicals as raw material production propylene comprises multiple stage radial fixed-bed reactor and inter-stage blender, described radial fixed-bed reactor comprises: cylindrical housings, the barrel type reactor that upper cover and low head form, barrel type reactor top and the bottom are respectively equipped with reaction gas inlet, reacting gas pre-distributor and product gas outlet, catalyst feeds and catalyst discharge port; Barrel type reactor internal placement has the porous wall inner core coaxial with cylindrical housings and porous wall urceolus, the outside runner of reacting gas is formed between porous wall urceolus and cylindrical housings, porous wall inner core and product gas outlet form reacting gas center flow channels, be catalyst filling zone between porous wall inner core and porous wall urceolus, top and the bottom, catalyst filling zone are respectively equipped with catalyst upper sealing plate and lower shrouding;
Described inter-stage blender is arranged between every two-stage radial fixed-bed reactor.
Described radial fixed-bed reactor reaction gases pre-distributor is connected with reaction gas inlet in reactor head, and reacting gas pre-distributor is porous wall cylinder, and perforate is uniform bore, and percent opening is 10 ~ 50%.
In described radial fixed-bed reactor, porous wall urceolus and the perforate of porous wall inner core can be uniform pore openings or non-homogeneous perforate, and percent opening is 10% ~ 50%.
The bed pressure drop of described catalyst in reactor filling area is 5 ~ 30kPa.
The thickness of bed layer of described radial fixed-bed reactor inner catalyst filling area is 200 ~ 800mm, and loaded catalyst increases progressively step by step.
Described multistage reactor number is 2 ~ 7.
A kind of multistage radial fixed-bed reaction method for taking oxygenatedchemicals as raw material production propylene is first through DME pre-reactor reaction methanol by methanol feedstock, the mixture of dimethyl ether and water, be N stock by this mixture flow point subsequently, the number of N is identical with radial fixed-bed reactor number, wherein first strand and process steam, first order radial fixed-bed reactor is injected after the mixture mixing of the part C2 that the outlet of N level radial fixed-bed reactor generates and each carbon number of C4 ~ C6 and alkane, the reaction logistics that M level radial fixed-bed reactor flows out and M stock methyl alcohol, as the charging of M+1 level radial fixed-bed reactor after the mixture hybrid cooling of dimethyl ether and water, wherein M is greater than 1 and is less than N-1.
Radial fixed-bed reactor inlet temperature at different levels is between 450 ~ 470 DEG C, and pressure is in gauge pressure 0.1 ~ 0.3 MPaG.
In radial fixed-bed reactor charging at different levels, the mass ratio of oxygenatedchemicals is identical with the mass ratio of radial fixed-bed reactor bed catalyst at different levels.
In the charging of first order radial fixed-bed reactor, the ratio of gross mass and the methyl alcohol in charging at different levels of the mixture of each carbon number of C2 and C4 ~ C6 and alkane and the gross mass of dimethyl ether is no more than 1.5:1.
The technique scheme that the present invention adopts, has following advantage:
Fixed bed reactors easily amplify in the industrial production, and no matter production scale is large or littlely can both to be well suitable for.
Compared with multi-layer fixed-bed axial flow reactor, owing to adopting porous wall urceolus as gas distributor, compared to gas, liquid two-phase nozzle, the uniform property of reacting gas in bed is improved, and avoids the generation of the bed hot localised points caused because distribution of gas is uneven.Meanwhile, because reactor catalyst thickness of bed layer is consistent, bed pressure drop is much smaller compared with axial flow reactor.
Compared with calandria type fixed bed, multistage multi-channel radial fixed bed and moving-burden bed reactor, structure of the present invention is more simple, and reactor manufacturing cost is lower.
Compared with fluidized-bed reactor, operating cost of the present invention reduces, the catalyst do not produced because catalyst granules is carried secretly by reacting gas seriously runs damage phenomenon, avoids the problems such as the pipeline wearing and tearing that cause containing a large amount of catalyst fines in reacting gas and piece-rate system blocking simultaneously.
Meanwhile, owing to adding a large amount of recycle hydrocarbons in first order charging, reactor temperature rise can be well controlled, and propene yield is owing to can increase 30%(carbon back compared to the reaction of one way preparing propylene from methanol adding of freshening) left and right.
Accompanying drawing explanation
Fig. 1 is the structural representation of radial fixed-bed reactor of the present invention;
Fig. 2 is radial fixed-bed reactor charging generalized section of the present invention.
Detailed description of the invention
As shown in Figure 1, a kind of for taking oxygenatedchemicals as the radial fixed-bed reactor that propylene produced by raw material, comprising: 1-reaction gas inlet, 2-reacting gas pre-distributor, 3-upper cover, 4-is containing catalyst upper sealing plate, 5-catalyst feeds, 6-cylindrical housings, 7-porous wall urceolus, 8-catalyst filling zone, 9-porous wall inner core, the outside runner of 10-reacting gas, shrouding under 11-catalyst, 12-reacting gas inner flow passage, 13-catalyst discharge port, 14-low head, 15-product gas outlet.
Because methanol partial pressure low in preparing propylene from methanol course of reaction is favourable to Propylene Selectivity, the operating pressure therefore in course of reaction should be in reduced levels, and this will ask reactor to be also low pressure drop reactor.In the present invention, reactor charge districts at different levels thickness is between 200 ~ 800mm, and bed pressure drop, between 5 ~ 30kPa, well meets the requirement of MTP reaction.Meanwhile, because the loadings of multistage reactor inner catalyst increases progressively step by step, under the prerequisite ensureing Catalyst packing consistency of thickness, loaded catalyst can be increased by the mode increasing height for reactor.But also it should be noted that, be not limited only to increase catalyst bed layer height, also can suitably increase catalyst bed layer thickness, but increment should not be excessive.
First order reactor feed gas is the mixed material having methyl alcohol, dimethyl ether, process steam, C2 and C4 ~ C6 alkene and alkane to form.Process steam add the dividing potential drop that can reduce methyl alcohol, dimethyl ether, improve Propylene Selectivity, the coking deactivation of catalyst surface can also be suppressed to a certain extent simultaneously.And the one side that adds of C2 and C4 ~ C6 alkene and alkane improves the thermal capacitance of reacting logistics, reduce the adiabatic temperature rise in course of reaction.Can also be reacted between C2 and C4 ~ C6 alkene propylene enhancing simultaneously, improves the ultimate yield of propylene.
embodiment 1
Unstrpped gas enters reactor from reaction gas inlet (1), and first distributes in advance through reacting gas pre-distributor (2).Following reaction gas enters the outside runner (10) of reacting gas, again after being axially uniformly distributed, enters catalyst filling zone (8) with ZSM-5 molecular sieve catalyst exposure through porous wall urceolus (7) and reacts.Product gas through porous wall inner core (9) outflow catalyst bed and from product gas outlet (15) discharge reactor after being collected in reacting gas inner flow passage (12).In this process, the flow direction of reacting gas enters bottom outflow from reactor top, is then flow from outside to inside at inside reactor.
3 fixed bed reactors series connection are adopted in the present embodiment, reaction temperature is 470 DEG C, reaction pressure is in gauge pressure 0.1 MPa, the Catalyst packing thickness of 3 reactors is 500 mm, the mass ratio of entrance recycle hydrocarbons and total methyl alcohol is 1.3:1, and the 3rd section of reactor outlet propylene carbon base absorption rate is 70.1%.
embodiment 2
Unstrpped gas enters reactor from reaction gas inlet (1), and first distributes in advance through reacting gas pre-distributor (2).Following reaction gas enters the outside runner (10) of reacting gas, again after being axially uniformly distributed, enters catalyst filling zone (8) with ZSM-5 molecular sieve catalyst exposure through porous wall urceolus (7) and reacts.Product gas through porous wall inner core (9) outflow catalyst bed and from product gas outlet (15) discharge reactor after being collected in reacting gas inner flow passage (12).In this process, the flow direction of reacting gas enters bottom outflow from reactor top, is then flow from outside to inside at inside reactor.
4 fixed bed reactors series connection are adopted in the present embodiment, reaction temperature is 470 DEG C, reaction pressure is in gauge pressure 0.1 MPa, the Catalyst packing thickness of 3 reactors is 400 mm, the mass ratio of entrance recycle hydrocarbons and total methyl alcohol is 1.1:1, and the 4th section of reactor outlet propylene carbon base absorption rate is 68.7%.
embodiment 3
Unstrpped gas enters reactor from reaction gas inlet (1), and first distributes in advance through reacting gas pre-distributor (2).Following reaction gas enters the outside runner (10) of reacting gas, again after being axially uniformly distributed, enters catalyst filling zone (8) with ZSM-5 molecular sieve catalyst exposure through porous wall urceolus (7) and reacts.Product gas through porous wall inner core (9) outflow catalyst bed and from product gas outlet (15) discharge reactor after being collected in reacting gas inner flow passage (12).In this process, the flow direction of reacting gas enters bottom outflow from reactor top, is then flow from outside to inside at inside reactor.
5 fixed bed reactors series connection are adopted in the present embodiment, reaction temperature is 470 DEG C, reaction pressure is in gauge pressure 0.1 MPa, the Catalyst packing thickness of 3 reactors is 300 mm, the mass ratio of entrance recycle hydrocarbons and total methyl alcohol is 1.3:1, and the 5th section of reactor outlet propylene carbon base absorption rate is 67.2%.
Claims (10)
1. the multistage radial fixed-bed reaction system for taking oxygenatedchemicals as raw material production propylene, it is characterized in that radial fixed-bed reaction system comprises multiple stage radial fixed-bed reactor and inter-stage blender, described radial fixed-bed reactor comprises: the barrel type reactor that cylindrical housings (6), upper cover (3) and low head (14) form, and barrel type reactor top and the bottom are respectively equipped with reaction gas inlet (1), reacting gas pre-distributor (2) and product gas outlet (15), catalyst feeds (5) and catalyst discharge port (13); Barrel type reactor internal placement has the porous wall inner core (9) coaxial with cylindrical housings and porous wall urceolus (7), the outside runner (10) of reacting gas is formed between porous wall urceolus (7) and cylindrical housings (6), porous wall inner core (9) and product gas outlet (15) form reacting gas center flow channels (12), be catalyst filling zone (8) between porous wall inner core (9) and porous wall urceolus (7), catalyst filling zone (8) top and the bottom are respectively equipped with catalyst upper sealing plate (4) and lower shrouding (11);
Described inter-stage blender is arranged between every two-stage radial fixed-bed reactor.
2. radial fixed-bed reactor according to claim 1, it is characterized in that: described radial fixed-bed reactor reaction gases pre-distributor (2) is connected with reaction gas inlet in reactor head, reacting gas pre-distributor (2) is porous wall cylinder, perforate is uniform bore, and percent opening is 10 ~ 50%.
3. radial fixed-bed reactor according to claim 1, is characterized in that: in described radial fixed-bed reactor, porous wall urceolus (7) and porous wall inner core (9) perforate can be uniform pore openings or non-homogeneous perforate, and percent opening is 10% ~ 50%.
4. radial fixed-bed reactor according to claim 1, is characterized in that: the bed pressure drop of described catalyst in reactor filling area (8) is 5 ~ 30kPa.
5. radial fixed-bed reactor according to claim 1, is characterized in that: the thickness of bed layer of described radial fixed-bed reactor inner catalyst filling area (8) is 200 ~ 800mm, and loaded catalyst increases progressively step by step.
6. radial fixed-bed reaction system according to claim 1, is characterized in that: described multistage reactor number is 2 ~ 7.
7. the multistage radial fixed-bed reaction method for taking oxygenatedchemicals as raw material production propylene, it is characterized in that methanol feedstock first through DME pre-reactor reaction methanol, the mixture of dimethyl ether and water, be N stock by this mixture flow point subsequently, the number of N is identical with radial fixed-bed reactor number, wherein first strand and process steam, first order radial fixed-bed reactor is injected after the mixture mixing of the part C2 that the outlet of N level radial fixed-bed reactor generates and each carbon number of C4 ~ C6 and alkane, the reaction logistics that M level radial fixed-bed reactor flows out and M stock methyl alcohol, as the charging of M+1 level radial fixed-bed reactor after the mixture hybrid cooling of dimethyl ether and water, wherein M is greater than 1 and is less than N-1.
8. reaction method according to claim 7, is characterized in that: described radial fixed-bed reactor inlet temperatures at different levels are between 450 ~ 470 DEG C, and pressure is in gauge pressure 0.1 ~ 0.3 MPaG.
9. reaction method according to claim 7, is characterized in that: in described radial fixed-bed reactor chargings at different levels, the mass ratio of oxygenatedchemicals is identical with the mass ratio of radial fixed-bed reactor bed catalyst at different levels.
10. reaction method according to claim 7, is characterized in that: in described first order radial fixed-bed reactor charging, the ratio of gross mass and the methyl alcohol in charging at different levels of the mixture of each carbon number of C2 and C4 ~ C6 and alkane and the gross mass of dimethyl ether is no more than 1.5:1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111992146A (en) * | 2020-08-27 | 2020-11-27 | 江苏正丹化学工业股份有限公司 | Axial and radial dehydrogenation reactor for vinyl toluene |
| CN114713146A (en) * | 2020-12-22 | 2022-07-08 | 中国石油化工股份有限公司 | Apparatus for producing epoxide and method for producing epoxide |
| CN114713145A (en) * | 2020-12-22 | 2022-07-08 | 中国石油化工股份有限公司 | Filling method of graded catalyst |
| CN115490566A (en) * | 2021-06-18 | 2022-12-20 | 中国石油化工股份有限公司 | Fixed bed reaction system and application thereof, and reaction regeneration method for preparing low-carbon olefin by converting oxygen-containing compound water material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN115490566A (en) * | 2021-06-18 | 2022-12-20 | 中国石油化工股份有限公司 | Fixed bed reaction system and application thereof, and reaction regeneration method for preparing low-carbon olefin by converting oxygen-containing compound water material |
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