CN102276387B - Low carbon olefin production method by oxygenated compounds - Google Patents
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- CN102276387B CN102276387B CN2010101997989A CN201010199798A CN102276387B CN 102276387 B CN102276387 B CN 102276387B CN 2010101997989 A CN2010101997989 A CN 2010101997989A CN 201010199798 A CN201010199798 A CN 201010199798A CN 102276387 B CN102276387 B CN 102276387B
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Abstract
The invention relates to a low carbon olefin production method by oxygenated compounds and mainly solves the problem of low yield of low carbon olefin during the production process of low carbon olefin. The low carbon olefin production method by oxygenated compounds in the invention mainly comprises the following steps of: (1) raw materials which mainly comprise methanol undergo heat exchange with a carbon deposition catalyst in an auxiliary reactor, enter into a main reactor and contact with an aluminosilicophosphate molecular sieve catalyst under effective conditions so as to produce a product containing low carbon olefin and simultaneously form the carbon deposition catalyst; (2) the carbon deposition catalyst enters into the auxiliary reactor from the main reactor and contacts with an ethanol-containing raw material to produce an ethene-containing product, which enters into the main reactor and simultaneously forms a catalyst to be generated; (3) the catalyst to be generated enters into a reactivator for regeneration. The technical scheme, by which the catalyst generated after the regeneration returns to the main reactor, greatly solves the above problem, and can be used in the industrial production of low carbon olefin.
Description
Technical field
The present invention relates to a kind of method of producing low-carbon olefins from oxygen-containing compound.
Technical background
Low-carbon alkene, promptly 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 of petroleum resources and higher price, 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 system ethene, propylene.Wherein, the alternative materials that is used for low-carbon alkene production that one class is important is an oxygenatedchemicals, for example alcohols (methyl alcohol, ethanol), ethers (dme, methyl ethyl ether), ester class (methylcarbonate, methyl-formiate) etc., these oxygenatedchemicalss can be transformed by coal, Sweet natural gas, biomass equal energy source.Some oxygenatedchemicals can reach fairly large production, as methyl alcohol, can be made by coal or Sweet natural gas, and technology is very ripe, can realize up to a million tonnes industrial scale.Because the popularity in oxygenatedchemicals source is added and is transformed the economy that generates low-carbon alkene technology, so by the technology of oxygen-containing compound conversion to produce olefine (OTO), particularly the technology by methanol conversion system alkene (MTO) is subjected to increasing attention.
In the US4499327 patent silicoaluminophosphamolecular molecular sieves catalyzer is applied to methanol conversion system olefin process and studies in great detail, think that SAPO-34 is the first-selected catalyzer of MTO technology.The SAPO-34 catalyzer has very high selectivity of light olefin, and activity is also higher, and can make methanol conversion is the degree that was less than in reaction times of low-carbon alkene 10 seconds, more even reach in the reaction time range of riser tube.
Announced among the US6166282 that a kind of methanol conversion is the technology and the reactor of low-carbon alkene, 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 significantly reduce.But there is the lower shortcoming of yield of light olefins in this method.
Announced among the CN1723262 that it is low-carbon alkene technology that the multiple riser reaction unit that has central catalyst return is used 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 product gas are separated.But there is the lower shortcoming of yield of light olefins in this method.
The method that relates to catalyzer coke content in a kind of MTO of control reactor reaction zone in US 20060025646 patents is the catalyzer part of inactivation to be sent into the breeding blanket make charcoal, and another part decaying catalyst turns back to reaction zone and continues reaction.But there is the lower shortcoming of yield of light olefins in this method.
CN 200910087868 has announced a kind of producing ethylene from dehydration of ethanol catalyzer, this catalyzer is the SAPO-34 molecular sieve of metal M n ion modification, be Mn/SAPO-34, with the morphine quinoline is that template is introduced the modified metal ion by direct synthesis technique and is prepared from before the molecular sieve crystallization, the gained molecular sieve is big crystal grain monocrystalline, can be directly used in fluidized-bed, the ethanol conversion height, selectivity of ethylene and purity are all very high.
Though ethanol conversion system ethene (ETO) technology has higher ethylene selectivity, and lower raw material dividing potential drop helps the raising of ethylene selectivity equally, but there are problems such as raw material production small scale, process economy in ETO technology at present, if ETO technology is relied on MTO technology, saved the construction cost of ETO process unit, had area development ethene, the propylene industry particularly suitable of a large amount of methyl alcohol and small amount of ethanol for some.
Though prior art can be carried out producing low-carbon olefins from oxygen-containing compound such as methyl alcohol or ethanol, but prior art is all less than the coupled problem that well solves MTO and ETO, simultaneously also do not have the lower problem of fine solution yield of light olefins, 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 method of new producing low-carbon olefins from oxygen-containing compound is provided.This method is used for the production of low-carbon alkene, has the yield of light olefins advantage of higher.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of method of producing low-carbon olefins from oxygen-containing compound, mainly may further comprise the steps: the raw material that (1) is mainly methyl alcohol is gone into main reactor with the carbon deposition catalyst heat exchange is laggard in auxiliary reactor, contact under condition for validity with the silicoaluminophosphamolecular molecular sieve catalyzer, generation comprises the product of low-carbon alkene, forms carbon deposition catalyst simultaneously; (2) described carbon deposition catalyst enters auxiliary reactor from the main reactor bottom, contacts with comprising the alcoholic acid raw material, generates the product that comprises ethene, enters main reactor, forms reclaimable catalyst simultaneously; (3) reclaimable catalyst enters revivifier regeneration, and the catalyzer that regeneration is finished returns main reactor.
In the technique scheme, described silicoaluminophosphamolecular molecular sieve is selected from least a among SAPO-18 or the SAPO-34, and preferred version is SAPO-34; Main reactor and auxiliary reactor are fluidized-bed; Described condition for validity: temperature of reaction is that 400 ℃～500 ℃, reaction pressure are counted 0.01～0.3MPa with gauge pressure, and gaseous line speed is 0.5～1.0 meter per second in the reactor; Described auxiliary reactor internal reaction condition: the mass ratio of ethanol charging and methanol feeding is between 0.1～0.6, and temperature of reaction is 300～420 ℃, and gaseous line speed is 0.3～0.8 meter per second; The methanol feedstock feeding temperature of described main reactor is between 180～300 ℃; Described carbon deposition catalyst carbon deposition quantity massfraction is between 2.0～5.0%; Described reclaimable catalyst carbon deposition quantity massfraction is between 2.5～6.0%; Described auxiliary reactor top links to each other with main reactor, and auxiliary reactor gas phase and carbon deposition catalyst are counter-current flow in catalyst stream is threaded a pipe.
The inventor is by discovering, the carbon deposition catalyst that forms in the methanol-to-olefins reaction process still keeps higher activity and selectivity, possesses the ability that transforms some low-carbon alcohol (as ethanol).Adopt method of the present invention, adopting the carbon deposition catalyst that forms in the MTO reaction to transform ethanol is ethene, and ethene enters the MTO reactor simultaneously, further propylene enhancing, and to have improved low-carbon alkene, the yield of propylene especially.
Adopt technical scheme of the present invention: described silicoaluminophosphamolecular molecular sieve is selected from least a among SAPO-18 or the SAPO-34, and preferred version is SAPO-34; Main reactor and auxiliary reactor are fluidized-bed; Described condition for validity: temperature of reaction is that 400 ℃～500 ℃, reaction pressure are counted 0.01～0.3MPa with gauge pressure, and gaseous line speed is 0.5～1.0 meter per second in the reactor; Described auxiliary reactor internal reaction condition: the mass ratio of ethanol charging and methanol feeding is between 0.1～0.6, and temperature of reaction is 300～420 ℃, and gaseous line speed is 0.3～0.8 meter per second; The methanol feedstock feeding temperature of described main reactor is between 180～300 ℃; Described carbon deposition catalyst carbon deposition quantity massfraction is between 2.0～5.0%; Described reclaimable catalyst carbon deposition quantity massfraction is between 2.5～6.0%; Described auxiliary reactor top links to each other with main reactor, auxiliary reactor gas phase and carbon deposition catalyst are counter-current flow in catalyst stream is threaded a pipe, methanol conversion reaches 99.82% (weight), ethanol conversion reaches 100% (weight), yield of ethene reaches 18.27% (weight), propene yield reaches 17.81% (weight), and the low-carbon alkene total recovery reaches 36.08% (weight), has obtained better technical effect.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
Among Fig. 1,1 for comprising the charging of alcoholic acid raw material; 2 is the raw material hot feed that comprises methyl alcohol; 3 is auxiliary reactor; 4 is main reactor; 5 is interior heat production coil pipe; 6 is the raw material cold feed that comprises methyl alcohol; 7 remove the revivifier pipeline for reclaimable catalyst; 8 is gas-solid cyclone separator; 9 is the main reactor settling section; 10 is the products export pipeline; 11 return the main reactor pipeline for regenerated catalyst.
The raw material that comprises methyl alcohol is gone into main reactor 4 with the carbon deposition catalyst heat exchange is laggard in auxiliary reactor 3, contact with the silicoaluminophosphamolecular molecular sieve catalyzer, generation comprises the product of low-carbon alkene, form carbon deposition catalyst simultaneously, carbon deposition catalyst enters auxiliary reactor 3 from main reactor 4 bottoms, contact with comprising the alcoholic acid raw material, generation comprises the product of ethene, enter main reactor 4, form reclaimable catalyst simultaneously, reclaimable catalyst enters revivifier regeneration by pipeline 7, and the catalyzer that regeneration is finished returns main reactor 4 by pipeline 11.
The invention will be further elaborated below by embodiment, but be not limited only to present embodiment.
Embodiment
[embodiment 1]
On reaction unit as shown in Figure 1, catalyzer adopts SAPO-34, main reactor and auxiliary reactor adopt fluidized-bed, main reactor employing purity is 99.5% methanol feeding, feeding temperature is 210 ℃, the main reactor reaction conditions is: temperature of reaction is that 450 ℃, reaction pressure are counted 0.01MPa with gauge pressure, and gaseous line speed is 0.7 meter per second in the reactor; Auxiliary reactor adopts the straight alcohol charging, and auxiliary reactor internal reaction condition: the mass ratio of ethanol charging and methanol feeding is 0.2, and temperature of reaction is 350 ℃, and gaseous line speed is 0.5 meter per second.The carbon deposition catalyst carbon deposition quantity is 2.5%, the reclaimable catalyst carbon deposition quantity is 2.97%, the main reactor outlet adopts the gas chromatographic analysis product to form, experimental result is: methanol conversion is 99.5% (weight), ethanol conversion is 100% (weight), yield of ethene is 17.38% (weight), and propene yield is 17.69% (weight).
[embodiment 2]
According to embodiment 1 described condition, just catalyzer adopts SAPO-18, and experimental result is: methanol conversion is 99.4% (weight), and ethanol conversion is 100% (weight), and yield of ethene is 15.98% (weight), and propene yield is 16.18% (weight).
[embodiment 3]
According to embodiment 1 described condition, main reactor employing purity is 99.5% methanol feeding, feeding temperature is 180 ℃, and the main reactor reaction conditions is: temperature of reaction is that 400 ℃, reaction pressure are counted 0.1MPa with gauge pressure, and gaseous line speed is 0.67 meter per second in the reactor; Auxiliary reactor adopts ethanol and methanol mixed charging, the mass ratio of ethanol and methanol feeding is 5.2 in the auxiliary reactor charging, the mass ratio of ethanol and methyl alcohol is 0.6 in the combined feed total feed, auxiliary reactor internal reaction condition: temperature of reaction is 420 ℃, and gaseous line speed is 0.8 meter per second.The carbon deposition catalyst carbon deposition quantity is 3.17%, the reclaimable catalyst carbon deposition quantity is 3.51%, and experimental result is: methanol conversion is 98.31% (weight), and ethanol conversion is 100% (weight), yield of ethene is 14.08% (weight), and propene yield is 16.92% (weight).
[embodiment 4]
According to embodiment 1 described condition, main reactor employing purity is 99.5% methanol feeding, feeding temperature is 300 ℃, and the main reactor reaction conditions is: temperature of reaction is that 500 ℃, reaction pressure are counted 0.3MPa with gauge pressure, and gaseous line speed is 0.5 meter per second in the reactor; Auxiliary reactor internal reaction condition: the mass ratio of ethanol charging and methanol feeding is 0.1, and temperature of reaction is 300 ℃, and gaseous line speed is 0.3 meter per second.The carbon deposition catalyst carbon deposition quantity is 4.98%, the reclaimable catalyst carbon deposition quantity is 5.94%, and experimental result is: methanol conversion is 99.76% (weight), and ethanol conversion is 100% (weight), yield of ethene is 15.23% (weight), and propene yield is 15.61% (weight).
[embodiment 5]
According to embodiment 1 described condition, main reactor employing purity is 99.5% methanol feeding, feeding temperature is 180 ℃, and the main reactor reaction conditions is: temperature of reaction is that 470 ℃, reaction pressure are counted 0.01MPa with gauge pressure, and gaseous line speed is 1.0 meter per seconds in the reactor; Auxiliary reactor internal reaction condition: the mass ratio of ethanol charging and methanol feeding is 0.4, and temperature of reaction is 367 ℃, and gaseous line speed is 0.59 meter per second.The carbon deposition catalyst carbon deposition quantity is 3.08%, the reclaimable catalyst carbon deposition quantity is 4.57%, and experimental result is: methanol conversion is 99.82% (weight), and ethanol conversion is 100% (weight), yield of ethene is 18.27% (weight), and propene yield is 17.81% (weight).
[comparative example 1]
According to embodiment 5 described conditions, auxiliary reactor is not set, methyl alcohol is laggardly gone into main reactor through being heated to 180 ℃, gaseous line speed is 0.86 meter per second in the main reactor, the reclaimable catalyst carbon deposition quantity is 3.23%, experimental result is: methanol conversion is 99.77% (weight), and yield of ethene is 16.86% (weight), and propene yield is 16.28% (weight).
Obviously, adopt method of the present invention, can reach the purpose that improves yield of light olefins, have bigger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (1)
1. the method for a producing low-carbon olefins from oxygen-containing compound mainly may further comprise the steps:
(1) raw material that is mainly methyl alcohol is gone into main reactor with the carbon deposition catalyst heat exchange is laggard in auxiliary reactor, contacts under condition for validity with the silicoaluminophosphamolecular molecular sieve catalyzer, generates the product that comprises low-carbon alkene, forms carbon deposition catalyst simultaneously;
(2) described carbon deposition catalyst enters auxiliary reactor from the main reactor bottom, contacts with comprising the alcoholic acid raw material, generates the product that comprises ethene, enters main reactor, forms reclaimable catalyst simultaneously;
(3) reclaimable catalyst enters revivifier regeneration, and the catalyzer that regeneration is finished returns main reactor;
Described silicoaluminophosphamolecular molecular sieve is selected from SAPO-34; Described main reactor and auxiliary reactor are fluidized-bed; Described condition for validity: temperature of reaction is that 400 ℃～500 ℃, reaction pressure are counted 0.01～0.3MPa with gauge pressure, and gaseous line speed is 0.5～1.0 meter per second in the reactor; Described auxiliary reactor internal reaction condition: the mass ratio of ethanol charging and methanol feeding is between 0.1～0.6, and temperature of reaction is 300～420 ℃, and gaseous line speed is 0.3～0.8 meter per second; The methanol feedstock feeding temperature of described main reactor is between 180～300 ℃; Described carbon deposition catalyst carbon deposition quantity massfraction is between 2.0～5.0%; Described reclaimable catalyst carbon deposition quantity massfraction is between 2.5～6.0%; Described auxiliary reactor top links to each other with main reactor, and auxiliary reactor gas phase and carbon deposition catalyst are counter-current flow in catalyst stream is threaded a pipe.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101270023A (en) * | 2008-04-11 | 2008-09-24 | 中国石油化工股份有限公司 | Method for improving selectivity of light olefin hydrocarbon |
| CN101270017A (en) * | 2008-04-11 | 2008-09-24 | 中国石油化工股份有限公司 | Process for producing light olefin hydrocarbon with oxygen-containing compound conversion |
| CN101270024A (en) * | 2008-04-11 | 2008-09-24 | 中国石油化工股份有限公司 | Method for preparing low carbon olefin hydrocarbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101270023A (en) * | 2008-04-11 | 2008-09-24 | 中国石油化工股份有限公司 | Method for improving selectivity of light olefin hydrocarbon |
| CN101270017A (en) * | 2008-04-11 | 2008-09-24 | 中国石油化工股份有限公司 | Process for producing light olefin hydrocarbon with oxygen-containing compound conversion |
| CN101270024A (en) * | 2008-04-11 | 2008-09-24 | 中国石油化工股份有限公司 | Method for preparing low carbon olefin hydrocarbon |
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