CN103121889A - Warm-taking method for preparing low-carbon olefin through conversion of oxygenated chemicals - Google Patents
Warm-taking method for preparing low-carbon olefin through conversion of oxygenated chemicals Download PDFInfo
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- CN103121889A CN103121889A CN2011103694379A CN201110369437A CN103121889A CN 103121889 A CN103121889 A CN 103121889A CN 2011103694379 A CN2011103694379 A CN 2011103694379A CN 201110369437 A CN201110369437 A CN 201110369437A CN 103121889 A CN103121889 A CN 103121889A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a warm-taking method for preparing low-carbon olefin through conversion of oxygenated chemicals, and mainly aims to solve the problems that the temperatures of a reactor and a regenerator are difficult to control, catalysts in a reaction region are not uniformly mixed and the like in the prior art. The warm-taking method for preparing the low-carbon olefin through conversion of the oxygenated chemicals mainly comprises the following steps of: contacting an oxygenated chemical raw material with a molecular sieve catalyst in a fluidized-bed reactor to generate low-carbon olefin and a spent catalyst; performing gas-solid separation on the generated low-carbon olefin and spent catalyst to ensure that the low-carbon olefin flows out from the top of the reactor, and the spent catalyst enters a precipitator; dividing the spent catalyst in the precipitator into at least three parts which respectively enter the reactor, the regenerator and an external warm-taking device; performing regeneration and degasification on the spent catalyst, and then dividing the spent catalyst into at least two parts which respectively enter the reactor and the external warm-taking device; and performing heat exchange on the catalyst in the external warm-taking device, and then dividing the catalyst into at least two parts which respectively enter the reactor and the regenerator. By adopting the technical scheme, the problems are well solved, and the warm-taking method can be used in industrial production for preparing the low-carbon olefin through conversion of the oxygenated chemicals.
Description
Technical field
The present invention relates to a kind of heat taking method of converting oxygen-containing compound to low-carbon olefins.
Background technology
Low-carbon alkene is defined as ethene and propylene here, is two kinds of important basic chemical industry raw materials, and its demand is in continuous increase.Ethene, propylene are mainly to make by petroleum path traditionally, but due to petroleum resources limited supply and higher price, the cost of being produced ethene, propylene by petroleum resources constantly increases.In recent years, people begin to greatly develop the substitute energy transformation technology, and as the technique of oxygen-containing compound conversion to produce olefine (OTO), oxygenatedchemicals comprises methyl alcohol, ethanol, dme, methyl ethyl ether, methylcarbonate etc.Have many technology to can be used to produce oxygenatedchemicals, raw material comprises coal, Sweet natural gas, biomass etc.As methyl alcohol, can be made by coal or Sweet natural gas, technique is very ripe, can realize the industrial scale of up to a million tonnes.Popularity due to the oxygenatedchemicals source, add and transform the economy that generates low-carbon alkene technique, so by the technique of oxygen-containing compound conversion to produce olefine (OTO), particularly the technique by preparing olefin by conversion of methanol (MTO) is subject to increasing attention.
In US 4499327 patents, silicoaluminophosphamolecular molecular sieve catalyst is applied to preparing olefin by conversion of methanol technique and studies in great detail, think that SAPO-34 is the first-selected catalyzer of MTO technique.The SAPO-34 catalyzer has very high selectivity of light olefin, and activity is also higher, and can make methanol conversion is reaction times of low-carbon alkene to be less than the degree of 10 seconds, more even reaches in the reaction time range of riser tube.
The method that relates to catalyzer coke content in a kind of MTO of control reactor reaction zone in the US20060025646 patent 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.
Technology and reactor that a kind of oxygenate conversion is low-carbon alkene have been announced in US 6166282, adopt fast fluidized bed reactor, gas phase is after the lower Mi Xiangfanyingqu reaction of gas speed is completed, 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.Due to reaction after product gas and catalyzer sharp separation, effectively prevented the generation of secondary reaction.
Known in the field, adhere to a certain amount of carbon deposit on the SAPO-34 catalyzer, be conducive to the selectivity of light olefin that keeps higher, and the agent of MTO technique alcohol is than very little, coking yield is lower, realize larger, hold manageable catalyst recirculation amount, just need in the breeding blanket, the coke content on catalyzer be controlled at certain level, and then reach the purpose of the average coke content of control reaction zone inner catalyst.Therefore, it is crucial how the average coke content of the catalyzer in reaction zone being controlled at certain level in the MTO technology.Methyl alcohol or dimethyl ether conversion are that the reaction of low-carbon alkene belongs to strong exothermal reaction, and heat how to take reaction away becomes a problem.The present invention adopts reactor and revivifier to share the mode of a heat collector, has solved targetedly this problem.
Summary of the invention
Technical problem to be solved by this invention is the problems such as the reactor that exists in prior art and the bad control of regenerator temperature, reaction zone catalyst mix be inhomogeneous, and a kind of heat taking method of new converting oxygen-containing compound to low-carbon olefins is provided.The method is used for the production of low-carbon alkene, has that reactor and regenerator temperature are controlled well, the uniform advantage of reaction zone catalyst mix.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows, a kind of heat taking method of converting oxygen-containing compound to low-carbon olefins, mainly comprise the following steps: oxygen-containing compound material contacts with molecular sieve catalyst in fluidized-bed reactor, generates the product stream I that comprises low-carbon alkene and reclaimable catalyst; The product stream I is after gas solid separation, and the gas-phase product that contains low-carbon alkene flows out from reactor head, and reclaimable catalyst enters settling vessel; In settling vessel, reclaimable catalyst is divided into three parts at least, and first part enters fluidized-bed reactor through the circulation inclined tube, and second section enters revivifier through inclined tube to be generated, and third part enters external warmer; Reclaimable catalyst forms regenerated catalyst after entering revivifier regeneration, and regenerated catalyst is divided into two portions at least after degassed, and first part enters fluidized-bed reactor through regenerator sloped tube, and second section enters external warmer; At least be divided into two portions after catalyzer in external warmer and heat transferring medium heat exchange, First enters fluidized-bed reactor, and second section enters revivifier.
In technique scheme, described oxygenatedchemicals is at least a in methyl alcohol or dme; Described molecular sieve comprises and is selected from least a in SAPO-5, SAPO-11, SAPO-18, SAPO-20, SAPO-34, SAPO-44 or SAPO-56.Described oxygenatedchemicals is methyl alcohol; Molecular screening is from SAPO-34.Reclaimable catalyst is in mass flux ratio first part in described settling vessel: second section: third part=0.01～100: 1: 0.01～100; Regenerated catalyst is degassed rear in mass flux ratio first part: second section=1: 0.01～100; Catalyzer in external warmer after heat-obtaining is in mass flux ratio first part: second section=1: 0.01～100.Reclaimable catalyst is in mass flux ratio first part in described settling vessel: second section: third part=1～20: 1: 0.1～10; Regenerated catalyst is degassed rear in mass flux ratio first part: second section=1: 0.1～10; Catalyzer in external warmer after heat-obtaining is in mass flux ratio first part: second section=1: 0.1～10.Adopt cyclonic separator to carry out gas solid separation to the product stream I.
Adopt method of the present invention, have the following advantages: (1) reactor and revivifier share an external warmer, have reduced equipment investment, save cost of investment; (2) the heat-obtaining load can be controlled flexibly, by adjusting external warmer to the flow of reactor and revivifier, reactor and regenerator temperature can be adjusted flexibly respectively; (3) catalyzer with respect to circulation inclined tube and regenerator sloped tube mixes in reactor, reclaimable catalyst and regenerated catalyst mix more even at external warmer, can be used as the catalyst charge supplementary means, in reactor, carbon deposited catalyst and temperature distribution are more even, are conducive to improve the selectivity of low-carbon alkene; (4) temperature controlling range of external warmer is large, and reactor and regenerator temperature have wider adjustment space.
Adopt technical scheme of the present invention: the oxygenatedchemicals in raw material is methyl alcohol, and SAPO type molecular screening is from the SAPO-34 molecular sieve; Reclaimable catalyst is in mass flux ratio first part in settling vessel: second section: third part=0.01～100: 1: 0.01～100; Regenerated catalyst is degassed rear in mass flux ratio first part: second section=1: 0.01～100; Catalyzer in external warmer after heat-obtaining is in mass flux ratio first part: second section=1: 0.01～100; The stream I gas solid separation adopts cyclonic separator, and the carbon base absorption rate massfraction of ethene+propylene reaches as high as 83.7% weight, has obtained technique effect preferably.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the invention.
In Fig. 1,1 is settling vessel; 2 is reactor; 3 is revivifier; 4 is external warmer; 5 is stripper; 6 is feed line; 7 is the regenerating medium pipeline; 8 are the circulation inclined tube; 9 is regenerator sloped tube; 10 are the negate inclined tube; 11 is inclined tube to be generated; 12 for getting inclined tube again; 13 are the heavy inclined tube of getting; 14 get inclined tube for vapour; 15 is product gas outlet; 16 is exhanst gas outlet; 17 is the heat transferring medium pipeline; 18 is cyclonic separator.
The oxygenatedchemicals of feed line 6 enters from fluidized-bed reactor 2 bottoms, contact with the catalyzer of circulation inclined tube 8, regenerator sloped tube 9, negate inclined tube 10, generation comprises gas product and the reclaimable catalyst of low-carbon alkene, gas product and reclaimable catalyst are after cyclonic separator 18 sharp separation, gas product goes separation system from product gas outlet 15, and reclaimable catalyst enters settling vessel 1; The interior reclaimable catalyst of settling vessel 1 is divided into three parts, and first part is through circulation inclined tube 8 Returning reactors 2, and second section removes revivifier 3 through pipeline 11 to be generated, and third part is got inclined tube 13 and entered external warmer 4 through heavy; The regenerating medium of regenerating medium pipeline 7 enters and enters stripper 5 revivifier 3 bottoms contact regeneration with the catalyzer of getting again inclined tube 12 with inclined tube 11 to be generated after, and the flue gas of formation is discharged from exhanst gas outlet 16; Catalyzer in stripper 5 is divided into two portions after stripping, first part gets inclined tube 14 through vapour and enters external warmer 4, and second section enters reactor 2 through regenerator sloped tube 9; Be divided into two portions after catalyzer in external warmer 4 and the heat transferring medium heat exchange in heat transferring medium pipeline 17, first part enters reactor 2 through negate inclined tube 10, and second section enters revivifier 3 through getting inclined tube 12 again.
The invention will be further elaborated below by embodiment, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
On reaction unit as shown in Figure 1, reactor adopts fast fluidized bed, and revivifier adopts turbulent bed, temperature of reaction is 450 ℃, and regeneration temperature is 650 ℃, is 0.01MPa in gauge pressure reaction and regeneration pressure, raw material adopts methyl alcohol, and regenerating medium is air, and the heat-obtaining medium is water.The coke content massfraction of controlling reclaimable catalyst is about 5.9%, and the coke content massfraction of regenerated catalyst is about 0.5%, and on catalyzer, Infrared Carbon-sulphur high speed analysis instrument is adopted in the analysis of carbon content.Reclaimable catalyst in settling vessel is controlled to be first part in mass flux ratio: second section: third part=20: 1: 0.5, be controlled to be first part in mass flux ratio after regenerated catalyst is degassed: second section=1: 0.5, the external warmer inner catalyst is controlled to be first part in mass flux ratio: second section=1: 1 makes system run all right, controls conveniently.Catalyzer adopts the SAPO-34 modified catalyst of spray-dried moulding.The reactor outlet product adopts online gas chromatographic analysis, and experimental result: the carbon base absorption rate massfraction of ethene+propylene is 81.5%.
[embodiment 2～8]
According to the described condition of embodiment 1, just change the mass flux ratio of reclaimable catalyst each several part in settling vessel, experimental result sees Table 1.
Table 1
[embodiment 9～13]
According to the described condition of embodiment 1, just change the mass flux ratio of the degassed rear each several part of regenerated catalyst, experimental result sees Table 2.
Table 2
[embodiment 14～18]
According to the described condition of embodiment 1, just change the mass flux ratio of external warmer inner catalyst each several part, experimental result sees Table 3.
Table 3
[embodiment 19～21]
According to the described condition of embodiment 1, just change the molecular sieve catalyst type, experimental result sees Table 4.
Table 4
[embodiment 22]
According to the described condition of embodiment 1, just change molecular sieve catalyst, mixed and go out experimental result according to the ratio of 1: 1 by SAPO-11 and SAPO-56: the carbon back massfraction yield of ethene+propylene is 33.9%.
[comparative example 1～3]
Reaction unit is changed, and reactor utilizes an external warmer heat-obtaining, and revivifier utilizes another external warmer heat-obtaining, and all according to embodiment 7,11,14 described conditions, experimental result sees Table 5 for all the other.
Table 5
Obviously, adopt method of the present invention, reactor and regenerator temperature are controlled well, saved equipment, and effectively improved oxygenatedchemicals transform the yield of producing light olefins under molecular sieve catalyst exists, have larger technical superiority, can be used in the industrial production of low-carbon alkene.
Claims (6)
1. the heat taking method of a converting oxygen-containing compound to low-carbon olefins mainly comprises the following steps:
A) oxygen-containing compound material contacts with molecular sieve catalyst in fluidized-bed reactor, generates the product stream I that comprises low-carbon alkene and reclaimable catalyst;
B) the product stream I is after gas solid separation, and the gas-phase product that contains low-carbon alkene flows out from reactor head, and reclaimable catalyst enters settling vessel;
C) in settling vessel, reclaimable catalyst is divided into three parts at least, and first part enters fluidized-bed reactor through the circulation inclined tube, and second section enters revivifier through inclined tube to be generated, and third part enters external warmer;
D) reclaimable catalyst forms regenerated catalyst after entering revivifier regeneration, and regenerated catalyst is divided into two portions at least after degassed, and first part enters fluidized-bed reactor through regenerator sloped tube, and second section enters external warmer;
E) be divided at least two portions after the catalyzer in external warmer and heat transferring medium heat exchange, First enters fluidized-bed reactor, and second section enters revivifier.
2. a kind of heat taking method of converting oxygen-containing compound to low-carbon olefins according to claim 1 is characterized in that described oxygenatedchemicals is at least a in methyl alcohol or dme; Described molecular sieve comprises and is selected from least a in SAPO-5, SAPO-11, SAPO-18, SAPO-20, SAPO-34, SAPO-44 or SAPO-56.
3. a kind of heat taking method of converting oxygen-containing compound to low-carbon olefins according to claim 2, is characterized in that described oxygenatedchemicals is methyl alcohol; Molecular screening is from SAPO-34.
4. a kind of heat taking method of converting oxygen-containing compound to low-carbon olefins according to claim 1 is characterized in that in described settling vessel that reclaimable catalyst is in mass flux ratio first part: second section: third part=0.01～100: 1: 0.01～100; Regenerated catalyst is degassed rear in mass flux ratio first part: second section=1: 0.01～100; Catalyzer in external warmer after heat-obtaining is in mass flux ratio first part: second section=1: 0.01～100.
5. a kind of heat taking method of converting oxygen-containing compound to low-carbon olefins according to claim 4 is characterized in that in described settling vessel that reclaimable catalyst is in mass flux ratio first part: second section: third part=1～20: 1: 0.1～10; Regenerated catalyst is degassed rear in mass flux ratio first part: second section=1: 0.1～10; Catalyzer in external warmer after heat-obtaining is in mass flux ratio first part: second section=1: 0.1～10.
6. a kind of heat taking method of converting oxygen-containing compound to low-carbon olefins according to claim 1, is characterized in that adopting cyclonic separator to carry out gas solid separation to the product stream I.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10040045B2 (en) | 2014-07-31 | 2018-08-07 | Uop Llc | FCC units, separation apparatuses, and methods for separating regenerated catalyst |
| CN113457586A (en) * | 2021-07-05 | 2021-10-01 | 中国石油化工股份有限公司 | External heating fluidized bed reactor and method for carbon monoxide isothermal transformation |
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| CN101293804A (en) * | 2007-04-28 | 2008-10-29 | 中国石油化工股份有限公司 | Fluidizer and method for preparing ethylene with ethanol dehydration |
| CN101293803A (en) * | 2008-04-11 | 2008-10-29 | 中国石油化工股份有限公司 | Method for converting oxygen-containing compounds into low carbon olefin hydrocarbon |
| CN101333142A (en) * | 2008-07-08 | 2008-12-31 | 中国石油化工股份有限公司 | Starting method of reaction-regenerative device for preparing low carbon olefin form methanol |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101293804A (en) * | 2007-04-28 | 2008-10-29 | 中国石油化工股份有限公司 | Fluidizer and method for preparing ethylene with ethanol dehydration |
| CN101293803A (en) * | 2008-04-11 | 2008-10-29 | 中国石油化工股份有限公司 | Method for converting oxygen-containing compounds into low carbon olefin hydrocarbon |
| CN101333142A (en) * | 2008-07-08 | 2008-12-31 | 中国石油化工股份有限公司 | Starting method of reaction-regenerative device for preparing low carbon olefin form methanol |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10040045B2 (en) | 2014-07-31 | 2018-08-07 | Uop Llc | FCC units, separation apparatuses, and methods for separating regenerated catalyst |
| CN113457586A (en) * | 2021-07-05 | 2021-10-01 | 中国石油化工股份有限公司 | External heating fluidized bed reactor and method for carbon monoxide isothermal transformation |
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Application publication date: 20130529 |