CN102875281B - Method for catalytically converting methanol to low-carbon olefins - Google Patents
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Abstract
The invention relates to a method for catalytically converting methanol to low-carbon olefins, mainly solving the problem of low yield of low-carbon olefins in the prior art. The method disclosed herein comprises the following steps: (a) letting a raw material mainly comprising methanol enter into a downer reaction zone, contact the raw material with a catalyst, letting the generated gas-phase flow and the catalyst enter into a rough-cut cyclone, letting the gas-phase flow enter into a separation section through a gas-phase outlet of a cyclone separator, separating to obtain low-carbon olefins and a C4 or higher hydrocarbon flow, wherein the gas-phase outlet of the rough-cut cyclone is connected with the inlet of the cyclone separator in a disengager; (b) letting the catalyst separated by the rough-cut cyclone and the cyclone separator enter into a regenerator through a regeneration standpipe, letting a regeneration catalyst enter into a riser reaction zone through a regeneration inclined pipe to contact with the C4 or higher hydrocarbon flow, and letting the generated gas-phase flow and the catalyst enter into a gas-solid distribution zone. The method disclosed herein well solves the problems and can be used in the industrial production of low-carbon olefins.
Description
Technical field
The present invention relates to a kind of method that methanol oxidation is converted into low-carbon alkene.
Technical background
Low-carbon alkene, i.e. ethene and propylene, be two kinds of important basic chemical industry raw materials, its demand is in continuous increase.Usually, ethene, propylene are produced by petroleum path, but due to the limited supply of petroleum resources and higher price, produce ethene by petroleum resources, the cost of propylene constantly increases.In recent years, people start to greatly develop the technology that alternative materials transforms ethene processed, propylene.Wherein, one class important for low-carbon alkene produce alternative materials be 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, and as methyl alcohol, can be obtained by coal or Sweet natural gas, technique is very ripe, can realize the industrial scale of up to a million tonnes.Due to the popularity in oxygenatedchemicals source, add the economy transforming and generate low-carbon alkene technique, so by the technique of oxygen-containing compound conversion to produce olefine (OTO), be particularly subject to increasing attention by the technique of preparing olefin by conversion of methanol (MTO).
Be applied to preparing olefin by conversion of methanol technique to silicoaluminophosphamolecular molecular sieve catalyst in US4499327 patent to study 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, methanol conversion can be made to be less than the degree of 10 seconds in reaction times of low-carbon alkene, more even reach in the reaction time range of riser tube.
Technology and reactor that a kind of methanol conversion is low-carbon alkene is disclosed in US 6166282, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu of gas speed has reacted, after rising to the fast subregion that internal diameter diminishes rapidly, special gas-solid separation equipment initial gross separation is adopted to go out most entrained catalyst.Due to reaction after product gas and catalyzer sharp separation, effectively prevent the generation of secondary reaction.Through analog calculation, compared with traditional bubbling fluidization bed bioreactor, needed for this fast fluidized bed reactor internal diameter and catalyzer, reserve all greatly reduces.But in the method, low-carbon alkene carbon base absorption rate is generally all about 77%, there is the problem that yield of light olefins is lower.
The multiple riser reaction unit disclosed in CN 1723262 with central catalyst return is low-carbon alkene technique for oxygenate conversion, this covering device comprises multiple riser reactor, gas solid separation district, multiple 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, low-carbon alkene carbon base absorption rate is generally all between 75 ~ 80%, there is the problem that yield of light olefins is lower equally.
All there is the lower problem of yield of light olefins in prior art, the present invention solves this problem targetedly.
Summary of the invention
Technical problem to be solved by this invention is the problem that the yield of light olefins that exists in prior art is lower, provides a kind of new methanol oxidation to be converted into the method for low-carbon alkene.The method is used for, in the production of low-carbon alkene, having the advantage that yield of light olefins is higher.
For solving the problem, the technical solution used in the present invention is as follows: a kind of methanol oxidation is converted into the method for low-carbon alkene, comprise the following steps: after the raw material that (a) is mainly methyl alcohol enters gas-solid distribution zone, enter down-flow fluidized bed using ECT reaction zone, with the catalyst exposure comprising sial phosphorus molecular sieve, generation comprises low-carbon alkene, the gaseous stream of C 4 olefin and catalyzer enter and slightly revolve, slightly revolve gaseous phase outlet to connect with the cyclone inlet in settling vessel, described gaseous stream enters centrifugal station from cyclonic separator gaseous phase outlet, be separated carbon more than four hydrocarbon stream obtaining low-carbon alkene product and comprise C 4 olefin, b () is slightly revolved the isolated catalyzer with cyclonic separator and enter revivifier by regeneration standpipe after sedimentation, stripping, catalyzer after regeneration enters riser reaction zone through regenerator sloped tube, contact with described carbon more than four hydrocarbon stream comprising C 4 olefin, the gaseous stream of generation and catalyzer enter gas-solid distribution zone.
In technique scheme, described in comprise C 4 olefin mass content in carbon more than four hydrocarbon stream of C 4 olefin and be greater than 75%; Described sial phosphorus molecular sieve comprises SAPO-34; Described riser reaction zone reaction conditions is: temperature of reaction is 500 ~ 600 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 4 ~ 12 meter per seconds; Down-flow fluidized bed using ECT reaction zone reaction conditions is: temperature of reaction is 430 ~ 530 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 5 ~ 10 meter per seconds; Described regenerated catalyst average product carbon amounts massfraction is 0.01 ~ 0.5%; Described revivifier and settling vessel coaxially arranged, revivifier is positioned at below settling vessel; Described gas-solid distribution zone is positioned at above described down-flow fluidized bed using ECT reaction zone, and the gaseous stream come from riser reaction zone and catalyzer enter down-flow fluidized bed using ECT reaction zone with described methanol feedstock after gas-solid distribution zone mixes; At least one position that described riser reaction zone axial direction due separates arranges opening for feed, and institute enters material and comprises methyl alcohol.
The method of calculation of average coke content of the present invention are that carbon deposit quality on catalyzer is divided by described catalyst quality.Carbon deposit measuring method on catalyzer is as follows: by the comparatively uniform catalyst mix with carbon deposit of mixing, then the band C catalyst of 0.1 ~ 1 gram is weighed, be put in pyrocarbon analyser and burn, by the carbonic acid gas quality that infrared analysis burning generates, thus obtain the carbonaceous amount on catalyzer.
The preparation method of sial phosphorus molecular sieve of the present invention is: first prepare molecular sieve precursor, is 0.03 ~ 0.6R by mol ratio: (Si 0.01 ~ 0.98: Al 0.01 ~ 0.6: P 0.01 ~ 0.6): 2 ~ 500H
2o, wherein R represents template, and template is triethylamine, constitutive material mixed solution, obtains at the temperature of 100-250 DEG C after the crystallization of 1 ~ 10 hour; Again, after molecular sieve precursor, phosphorus source, silicon source, aluminium source, template, water etc. being mixed according to certain ratio, at 110 ~ 260 DEG C, hydrothermal crystallizing, after at least 0.1 hour, finally obtains SAPO molecular sieve.Mixed with the binding agent of required ratio by the molecular sieve of preparation, after the operation steps such as spraying dry, roasting, obtain final SAPO catalyzer, the weight percentage of binding agent in molecular sieve is between 10 ~ 90%.
In the present invention, slightly revolve and refer to and be positioned at riser tube or down-flow fluidized bed using ECT outlet can realize the primary cyclone of gas-solid sharp separation, due to its separation efficiency lower (generally between 70 ~ 90%), therefore those skilled in the art is generally simply referred to as " slightly revolving ".And down-flow fluidized bed using ECT refers to that solid particulate presents the tubular reactor of flow pattern from top to bottom under solid particulate self gravitation or airflow acting force.Gas-solid distribution zone is generally positioned at descending-bed reactor inlet end, enters down-flow fluidized bed using ECT after gas, the mixing of Gu Gai district through descending-bed reactor inlet distributor, its effect be ensure descending-bed reactor inlet end gas, solid distribute all with, raising gas-solid contact efficiency.
Adopt method of the present invention, arrange two reaction zones, carbon more than four hydrocarbon being mainly used in converting methanol reaction generation in riser reaction zone is low-carbon alkene, and the main converting methanol in down-flow fluidized bed using ECT reaction zone is low-carbon alkene.Be high temperature, highly active regenerated catalyst in riser reaction zone, can ensure higher C 4 olefin transformation efficiency, the high linear speed of riser tube can improve selectivity of light olefin again, and in riser tube, C 4 olefin scission reaction can be again the pre-carbon distribution of regenerated catalyst simultaneously.And in down-flow fluidized bed using ECT reaction zone be the catalyzer of pre-carbon distribution, there is the advantage that selectivity is higher, down-flow fluidized bed using ECT Gas-particle Flows be similar to the advantage of plug flow favourable improve selectivity of light olefin.In addition, down-flow fluidized bed using ECT outlet connects slightly revolves, and slightly revolve the entrance that gaseous phase outlet connects cyclonic separator, being separated as early as possible of gaseous stream and catalyzer can be ensured, avoid overstand in settling vessel to cause the generation of some side reaction, arrange at least one opening for feed simultaneously on the axial direction due of riser reaction zone, institute enters material and comprises methyl alcohol, the effect reducing gaseous stream dividing potential drop in riser tube can be played, thus reach the object improving selectivity of light olefin.Therefore, adopt method of the present invention, the object improving yield of light olefins can be reached.
Adopt technical scheme of the present invention: described in comprise C 4 olefin mass content in carbon more than four hydrocarbon stream of C 4 olefin and be greater than 75%; Described sial phosphorus molecular sieve comprises SAPO-34; Described riser reaction zone reaction conditions is: temperature of reaction is 500 ~ 600 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 4 ~ 12 meter per seconds; Down-flow fluidized bed using ECT reaction zone reaction conditions is: temperature of reaction is 430 ~ 530 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 5 ~ 10 meter per seconds; Described regenerated catalyst average product carbon amounts massfraction is 0.01 ~ 0.5%; Described revivifier and settling vessel coaxially arranged, revivifier is positioned at below settling vessel; Described gas-solid distribution zone is positioned at above described down-flow fluidized bed using ECT reaction zone, and the gaseous stream come from riser reaction zone and catalyzer enter down-flow fluidized bed using ECT reaction zone with described methanol feedstock after gas-solid distribution zone mixes; At least one position that described riser reaction zone axial direction due separates arranges opening for feed, institute enters material and comprises methyl alcohol, low-carbon alkene carbon base absorption rate reaches 87.91% (weight), exceed than the low-carbon alkene carbon base absorption rate of prior art and can reach more than 5 percentage points, achieve good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the invention.
In Fig. 1,1 is regeneration air feed pipeline; 2 is plug valve under regeneration standpipe; 3 is revivifier; 4 is stripper; 5 is stripped vapor charging; 6 is regeneration standpipe; 7 is regenerator sloped tube; 8 is riser tube charging; 9 is riser reaction zone axial direction due opening for feed; 10 is riser reaction zone lower lift section; 11 is riser reaction zone; 12 is revivifier gas-solid cyclone separator; 13 is exhanst gas outlet; 14 is delivering vapor; 15 is product gas outlet; 16 is settling vessel; 17 for slightly to revolve; 18 is down-flow fluidized bed using ECT reaction zone; 19 is gas-solid distribution zone; 20 is methanol feeding; 21 is cyclonic separator in settling vessel.
The raw material being mainly methyl alcohol enters after gas-solid distribution zone 19 through pipeline 20 and enters down-flow fluidized bed using ECT reaction zone 18, with the catalyst exposure comprising sial phosphorus molecular sieve, generation comprises low-carbon alkene, the gaseous stream of C 4 olefin and catalyzer enter and slightly revolve 17, slightly revolve 17 gaseous phase outlets to connect with cyclonic separator 21 entrance in settling vessel 16, gaseous stream enters centrifugal station from cyclonic separator 21 gaseous phase outlet, be separated carbon more than four hydrocarbon stream obtaining low-carbon alkene product and comprise C 4 olefin, slightly revolve 17 and the isolated catalyzer of cyclonic separator 21 through sedimentation, revivifier 3 is entered by regeneration standpipe 6 after stripping, catalyzer after regeneration enters riser reaction zone 11 through regenerator sloped tube 7, contact with described carbon more than four hydrocarbon stream comprising C 4 olefin, the gaseous stream generated and catalyzer enter gas-solid distribution zone 19.
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, pure methanol feedstock enters after gas-solid distribution zone 19 through pipeline 20 and enters down-flow fluidized bed using ECT reaction zone 18, with SAPO-34 catalyst exposure, generation comprises low-carbon alkene, the gaseous stream of C 4 olefin and catalyzer enter and slightly revolve 17, slightly revolve 17 gaseous phase outlets to connect with cyclonic separator 21 entrance in settling vessel 16, gaseous stream enters centrifugal station from cyclonic separator 21 gaseous phase outlet, be separated carbon more than four hydrocarbon stream obtaining low-carbon alkene product and comprise C 4 olefin, slightly revolve 17 and the isolated catalyzer of cyclonic separator 21 through sedimentation, revivifier 3 is entered by regeneration standpipe 6 after stripping, catalyzer after regeneration enters riser reaction zone 11 through regenerator sloped tube 7, contact with described carbon more than four hydrocarbon stream comprising C 4 olefin, the gaseous stream generated and catalyzer enter gas-solid distribution zone 19.The massfraction of SAPO-34 catalyzer Middle molecule sieve is 40%, riser tube 11 charging is carbon more than four hydrocarbon stream comprising C 4 olefin, wherein C_4 hydrocarbon classical group prejudice table 1, C 4 olefin mass content is 75.33%, riser reaction zone 11 reaction conditions is: temperature of reaction is 500 DEG C, reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 4 meter per seconds; Down-flow fluidized bed using ECT reacts 18 reaction conditionss: temperature of reaction is 430 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 5 meter per seconds.Regenerated catalyst average product carbon amounts massfraction is 0.01%, revivifier 3 is coaxially arranged with settling vessel 16, revivifier 2 is positioned at below settling vessel 16, gas-solid distribution zone 19 is positioned at above down-flow fluidized bed using ECT reaction zone 18, enters down-flow fluidized bed using ECT reaction zone from the gaseous stream of riser reaction zone 11 and catalyzer with methanol feedstock after gas-solid distribution zone 19 mixes.Riser reaction zone 11 axial direction due arranges an opening for feed, and it is pure methyl alcohol that material enters in institute, and the methyl alcohol that described axial feed inlet enters and C 4 olefin mass ratio are 1: 2.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 83.68% (weight).
Table 1 C_4 hydrocarbon classical group becomes distribution
| Component | Massfraction, % |
| Trimethylmethane | 10.25 |
| Normal butane | 14.42 |
| Anti-2-butylene | 16.75 |
| 1-butylene | 25.17 |
| Iso-butylene | 4.48 |
| Along 2-butylene | 27.05 |
| 1.3-divinyl | 1.88 |
[embodiment 2]
According to the condition described in embodiment 1 and step, purity is that 81% methanol feedstock (all the other are water) enters after gas-solid distribution zone 19 through pipeline 20 and enters down-flow fluidized bed using ECT reaction zone 18.Riser tube 11 charging is carbon more than four hydrocarbon stream comprising C 4 olefin, and wherein C 4 olefin mass content is 88%, and riser reaction zone 11 reaction conditions is: temperature of reaction is 600 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 12 meter per seconds; Down-flow fluidized bed using ECT reacts 18 reaction conditionss: temperature of reaction is 530 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 10 meter per seconds.Regenerated catalyst average product carbon amounts massfraction is 0.5%, riser reaction zone 11 axial direction due arranges two opening for feeds, two opening for feeds lay respectively at 1/3/, 1/2 reaction zone At The Height bottom distance riser tube, to enter material be purity be 81% methyl alcohol, the methyl alcohol that described axial feed inlet enters and C 4 olefin mass ratio are 1: 1.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 85.71% (weight).
[embodiment 3]
According to the condition described in embodiment 1 and step, riser tube 11 charging is carbon more than four hydrocarbon stream comprising C 4 olefin, wherein C 4 olefin mass content is 88%, riser reaction zone 11 reaction conditions is: temperature of reaction is 550 DEG C, reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 7 meter per seconds; Down-flow fluidized bed using ECT reacts 18 reaction conditionss: temperature of reaction is 465 DEG C, and reaction pressure counts 0.01MPa with gauge pressure, and gas phase linear speed is 7 meter per seconds.Regenerated catalyst average product carbon amounts massfraction is 0.12%, riser reaction zone 11 axial direction due arranges three opening for feeds, three opening for feeds lay respectively at 1/3/, 1/2,2/3 reaction zone At The Height bottom distance riser tube, and the methyl alcohol that described axial feed inlet enters and C 4 olefin mass ratio are 1: 1.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 87.91% (weight).
[embodiment 4]
According to the condition described in embodiment 1 and step, riser tube 11 charging is carbon more than four hydrocarbon stream comprising C 4 olefin, wherein C 4 olefin mass content is 92%, riser reaction zone 11 reaction conditions is: temperature of reaction is 570 DEG C, reaction pressure counts 0.3MPa with gauge pressure, and gas phase linear speed is 5 meter per seconds; Down-flow fluidized bed using ECT reacts 18 reaction conditionss: temperature of reaction is 475 DEG C, and reaction pressure counts 0.3MPa with gauge pressure, and gas phase linear speed is 6 meter per seconds.Regenerated catalyst average product carbon amounts massfraction is 0.06%, riser reaction zone 11 axial direction due arranges three opening for feeds, three opening for feeds lay respectively at 1/3/, 1/2,2/3 reaction zone At The Height bottom distance riser tube, and the methyl alcohol that described axial feed inlet enters and C 4 olefin mass ratio are 1: 1.Reactor product adopts online gas chromatographic analysis, and low-carbon alkene carbon base absorption rate is 85.29% (weight).
[comparative example 1]
According to the condition described in embodiment 3 and step, just do not arrange riser reaction zone 11 axial feed inlet, all methanol feedstocks all enter down-flow fluidized bed using ECT reaction zone 18, and yield of light olefins is 86.98% (weight).
[comparative example 2]
According to the condition described in embodiment 3 and step, just down-flow fluidized bed using ECT reacts the gaseous phase outlet that the outlet of 18th district slightly revolves 17 and does not connect with cyclonic separator 21, and yield of light olefins is 87.07% (weight).
[comparative example 3]
According to the condition described in embodiment 3 and step, just down-flow fluidized bed using ECT reaction zone 18 is not set, methanol feedstock enters riser reaction zone 11 from pipeline 8, carbon more than four hydrocarbon stream comprising C 4 olefin generated does not enter riser reaction zone 11, riser reaction zone 11 outlet connects with settling vessel 16, and yield of light olefins is 82.87% (weight).
Obviously, adopt method of the present invention, the object improving yield of light olefins can be reached, there is larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (3)
1. methanol oxidation is converted into a method for low-carbon alkene, comprises the following steps:
Down-flow fluidized bed using ECT reaction zone is entered after a raw material that () is mainly methyl alcohol enters gas-solid distribution zone, with the catalyst exposure comprising sial phosphorus molecular sieve, generate and comprise low-carbon alkene, the gaseous stream of C 4 olefin and catalyzer and enter and slightly revolve, slightly revolve gaseous phase outlet to connect with the cyclone inlet in settling vessel, described gaseous stream enters centrifugal station from cyclonic separator gaseous phase outlet, is separated carbon more than four hydrocarbon stream obtaining low-carbon alkene product and comprise C 4 olefin;
B () is slightly revolved the isolated catalyzer with cyclonic separator and enter revivifier by regeneration standpipe after sedimentation, stripping, catalyzer after regeneration enters riser reaction zone through regenerator sloped tube, contact with described carbon more than four hydrocarbon stream comprising C 4 olefin, the gaseous stream of generation and catalyzer enter gas-solid distribution zone;
Described riser reaction zone reaction conditions is: temperature of reaction is 500 ~ 600 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 4 ~ 12 meter per seconds; Down-flow fluidized bed using ECT reaction zone reaction conditions is: temperature of reaction is 430 ~ 530 DEG C, and reaction pressure counts 0.01 ~ 0.3MPa with gauge pressure, and gas phase linear speed is 5 ~ 10 meter per seconds;
Describedly comprise C 4 olefin mass content in carbon more than four hydrocarbon stream of C 4 olefin and be greater than 75%;
Described revivifier and settling vessel coaxially arranged, revivifier is positioned at below settling vessel; Described gas-solid distribution zone is positioned at above described down-flow fluidized bed using ECT reaction zone, and the gaseous stream come from riser reaction zone and catalyzer enter down-flow fluidized bed using ECT reaction zone with described methanol feedstock after gas-solid distribution zone mixes; At least one position that described riser reaction zone axial direction due separates arranges opening for feed, and institute enters material and comprises methyl alcohol.
2. methanol oxidation is converted into the method for low-carbon alkene according to claim 1, it is characterized in that described sial phosphorus molecular sieve comprises SAPO-34.
3. methanol oxidation is converted into the method for low-carbon alkene according to claim 1, it is characterized in that described regenerated catalyst average product carbon amounts massfraction is 0.01 ~ 0.5%.
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| CN112705127B (en) * | 2019-10-24 | 2022-11-01 | 中国石油化工股份有限公司 | Reactor and method for producing low-carbon olefin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6166282A (en) * | 1999-08-20 | 2000-12-26 | Uop Llc | Fast-fluidized bed reactor for MTO process |
| CN101279877A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for increasing yield of ethylene and propone in conversion process of oxocompound |
| CN101270023B (en) * | 2008-04-11 | 2011-04-27 | 中国石油化工股份有限公司 | Method for improving yield of light olefin hydrocarbon |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6166282A (en) * | 1999-08-20 | 2000-12-26 | Uop Llc | Fast-fluidized bed reactor for MTO process |
| CN101279877A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for increasing yield of ethylene and propone in conversion process of oxocompound |
| CN101270023B (en) * | 2008-04-11 | 2011-04-27 | 中国石油化工股份有限公司 | Method for improving yield of light olefin hydrocarbon |
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