CN104628507B - By the method for preparing low-carbon olefin by using methanol - Google Patents
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Abstract
The present invention relates to a kind of methods by preparing low-carbon olefin by using methanol, mainly solve the problems, such as that yield of light olefins is low in the prior art.The present invention is by using mainly including the following steps that：(1) it is mainly that the raw material of methanol enters reactor A, is contacted with catalyst A, the hydrocarbon mixture that generation includes low-carbon alkene enters centrifugal station；(2) ethylene, propylene are isolated as product, it isolates C4~C6 hydrocarbon and enters reactor C, the hydrocarbon mixture of reactor C generations returns to the centrifugal station, it isolates more than C6 hydrocarbon and enters reactor B, the technical solution that the hydrocarbon mixture of reactor B generation returns to the centrifugal station preferably solves the above problem, available in the industrial production of low-carbon alkene.
Description
Technical field
The present invention relates to a kind of methods by preparing low-carbon olefin by using methanol.
Background technology
Low-carbon alkene, i.e. ethylene and propylene, are two kinds of important basic chemical industry raw materials, and demand is being continuously increased.One
As, ethylene, propylene are produced by petroleum path, but due to the limited supply of petroleum resources and higher price, by
Petroleum resources produce ethylene, the cost of propylene is continuously increased.In recent years, people start to greatly develop alternative materials conversion second processed
The technology of alkene, propylene.Wherein, a kind of important alternative materials for light olefin production are oxygenatedchemicals, such as alcohols
(methanol, ethyl alcohol), ethers (dimethyl ether, ethyl methyl ether), esters (dimethyl carbonate, methyl formate) etc., these oxygenatedchemicals can
To be come by energy conversions such as coal, natural gas, biomass.Certain oxygenatedchemicals can reach fairly large life
Production, such as methanol can be made by coal or natural gas, and technique is very ripe, can realize the production scale of 10,000 tons up to a hundred.Due to
The popularity in oxygenatedchemicals source, along with the economy for being converted into light olefin technique, so being turned by oxygenatedchemicals
The technique for changing alkene (OTO) processed, is particularly more and more paid attention to by the technique of preparing olefin by conversion of methanol (MTO).
Technology and reactor that a kind of oxide is converted into low-carbon alkene are disclosed in US6166282, using fast fluidization
Bed reactor, gas phase after rising to the fast subregion that internal diameter rapidly becomes smaller, are adopted after the completion of the relatively low Mi Xiangfanyingqu reactions of gas velocity
Go out most entrained catalyst with special gas-solid separation equipment initial gross separation.Since product gas after reaction and catalyst are quick
Separation, effectively prevents the generation of secondary response.It is calculated through simulation, compared with traditional bubbling fluidized bed reactor, this is fast
Reserve needed for fast fluidized-bed reactor internal diameter and catalyst greatly reduces.
The multiple riser reaction unit with central catalyst return is disclosed in CN1723262 for oxide to turn
Low-carbon alkene technique is turned to, which includes multiple riser reactors, gas solid separation area, multiple offset components etc., each
Riser reactor respectively has the port of injecting catalyst, is pooled to the Disengagement zone of setting, catalyst and product gas are separated.
But this method there are yield of light olefins it is relatively low the shortcomings that.
A kind of method of methanol production propylene is disclosed in EP0448000 and EP0882692, methanol is first converted into DME
And water, mixture is then transported to First reactor, and steam is added in into the reactor.Methanol in the first reactor
And (or) dimethyl ether or its mixture are contacted with catalyst and are reacted, catalyst is urged using the special ZSM-5 containing ZnO and CdO
Agent, 280~570 DEG C, 0.01~0.1MPa of pressure of reaction temperature, is prepared the product using propylene as main hydro carbons.It is heavier
Product such as C5 +Hydrocarbon continuation carries out reaction in second reactor and is converted into hydro carbons based on propylene, sends back to after cooling point
From device.Product is compressed, further refine after can obtain the chemical grade propylene that purity is 97%.But using multiple in the technique
Fixed bed reactors, due to the activity limitation of catalyst, it is therefore desirable to which frequent switching operates, and takes heat problem also very complicated.
US 20070083071 discloses the process of a kind of hydrocarbon catalytic pyrolysis production ethylene, propylene, and hydrocarbon raw material is being urged
Change in pyrolysis furnace and be converted into the product including low-carbon alkene, product stream is then separated into C2~C3 alkane by series of process
C2~C3 alkane is returned to tube cracking furnace and carries out thermal cracking by three kinds of hydrocarbon, C2~C3 alkene, C4+ hydrocarbon logistics, and the return of C4+ hydrocarbon is urged
Change pyrolysis furnace and carry out catalytic pyrolysis, finally obtain ethylene, the propylene product of higher yields.This method uses riser reactor,
Reactant residence time is shorter, and low-carbon alkene product once through yield is relatively low.
The prior art there are yield of light olefins it is relatively low the problem of.The present invention targetedly solves the problems, such as this.
Invention content
The technical problems to be solved by the invention are the problem of yield of light olefins in the prior art are not high, are provided
A kind of new method by preparing low-carbon olefin by using methanol.This method is used in the production of low-carbon alkene, has yield of light olefins
The advantages of higher.
To solve the above problems, the technical solution adopted by the present invention is as follows：A kind of method by preparing low-carbon olefin by using methanol,
It mainly includes the following steps that：(1) it is mainly that the raw material of methanol enters reactor A, is contacted with catalyst A, generation includes low-carbon alkene
The hydrocarbon mixture of hydrocarbon enters centrifugal station；(2) ethylene, propylene are isolated as product, C4~C6 hydrocarbon is isolated and enters reactor C,
The hydrocarbon mixture of reactor C generations returns to the centrifugal station, isolates more than C6 hydrocarbon and enters reactor B, reactor B generation mixes
It closes hydrocarbon and returns to the centrifugal station.
In above-mentioned technical proposal, the catalyst A includes ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio is 30~200, hydrogen
Shift index is less than 0.3；Catalyst B includes ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio is 10~80；Catalyst C includes
ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio is 10~100；The reactor A is fixed bed, moving bed or fluid bed；Reaction
Device B is fixed bed, moving bed or fluid bed；Reactor C is fluid bed；Alkene mass percentage is more than in C4~C6 hydrocarbon
50%；The centrifugal station isolates low-carbon alkanes as product or as steam crack material；Item is reacted in the reactor A
Part is：Reaction temperature is 400~550 DEG C, and reaction pressure is calculated as 0.01~0.3MPa with gauge pressure, and the gas phase residence time is 1~5
Second；Reaction condition is in reactor C：Reaction temperature is 550~700 DEG C, and reaction pressure is calculated as 0.01~0.3MPa, gas with gauge pressure
The phase residence time is 2~10 seconds；Reaction condition is in reactor B：Reaction temperature is 500~650 DEG C, and reaction pressure is in terms of gauge pressure
For 0.01~0.3MPa, the gas phase residence time is 1~8 second；The reactor A exports the carbon-based selection property amount of low-carbon alkene one way
Score is more than 50%；The vapor that mass fraction is 1~50% is added in the reactor B, C chargings.
Method known in the field, such as hydrothermal synthesis method may be used in ZSM-5 molecular sieve of the present invention, is made
It is standby, on the molecular sieve catalyst can selectivity carried metal, metal in the periodic table of elements I B, II B, V B, VI B,
At least one of VII B or VIII race, and side known in the field is can be used into the method on ZSM-5 molecular sieve in Metal Supported
Method, such as infusion process or coprecipitation.Fluid catalyst is such as prepared, after ZSM-5 molecular sieve prepares, binding agent is added in, makes
Molding is dried using spray drying process in mixed slurry, then by catalyst fines after molding be placed in roaster into
Row roasting, catalyst sample is obtained after cooling.SiO may be selected in binding agent2、Al2O3Deng.
Hydrogen transfer index of the present invention is defined as in product propylene and butylene in the weight divided by product of propane and butane
Weight.
Method using the present invention, methanol is converted into the hydrocarbon mixture including low-carbon alkene in reactor A, and hydrocarbon mixture is through dividing
From rear, ethylene, propylene are as product, and catalytic pyrolysis is to include low-carbon to the C4~C6 isolated under higher temperature in reactor C
The hydrocarbon mixture of alkene returns to centrifugal station, and catalytic pyrolysis at more than the C6 hydrocarbon separated temperature suitable in reactor B
It is the hydrocarbon mixture return centrifugal station for including low-carbon alkene.In addition, the alkane product that centrifugal station is separated, such as ethane, third
Alkane, butane etc. can be used as product, preferably as steam crack material, increasing output of ethylene, propylene.Therefore, side using the present invention
Method can achieve the purpose that improve yield of light olefins.
Technical solution using the present invention：The catalyst A includes ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio for 30~
200, hydrogen transfer index is less than 0.3；Catalyst B includes ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio is 10~80；Catalyst C
Including ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio is 10~100；The reactor A is fixed bed, moving bed or fluid bed；
Reactor B is fixed bed, moving bed or fluid bed；Reactor C is fluid bed；Alkene mass percentage in C4~C6 hydrocarbon
More than 50%；The centrifugal station isolates low-carbon alkanes as product or as steam crack material；It is anti-in the reactor A
The condition is answered to be：Reaction temperature is 400~550 DEG C, and reaction pressure is calculated as 0.01~0.3MPa with gauge pressure, and the gas phase residence time is 1
~5 seconds；Reaction condition is in reactor C：Reaction temperature is 550~700 DEG C, reaction pressure is calculated as 0.01 with gauge pressure~
0.3MPa, gas phase residence time are 2~10 seconds；Reaction condition is in reactor B：Reaction temperature is 500~650 DEG C, reaction pressure
Power is calculated as 0.01~0.3MPa with gauge pressure, and the gas phase residence time is 1~8 second；The reactor A outlet low-carbon alkene one way is carbon-based
Selective mass fraction is more than 50%；The vapor that mass fraction is 1~50%, low-carbon are added in the reactor B, C chargings
Alkene carbon base absorption rate can reach 73.38% weight, achieve preferable technique effect.
Description of the drawings
Fig. 1 is the flow diagram of the method for the invention.
In Fig. 1,1 is methanol feedstock；2 be reactor A；3 be centrifugal station；4 be low-carbon alkene product；5 be alkane；6 are
C4~C6 hydrocarbon；7 be reactor C；8 be other products；9 be more than C6 hydrocarbon；10 be reactor B.
Predominantly the raw material 1 of methanol enters reactor A, is contacted with catalyst A, generation include the hydrocarbon mixture of low-carbon alkene into
Enter centrifugal station 3, isolate ethylene, propylene product 4, isolate C4~C6 hydrocarbon 6 and enter reactor C7, reactor C7 generations mix
It closes hydrocarbon and returns to the centrifugal station 3, isolate more than C6 hydrocarbon 9 and enter reactor B 10, the hydrocarbon mixture that reactor B 10 generates returns
The centrifugal station 3.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
【Embodiment 1】
In reaction system as shown in Figure 1, the methanol feedstock that purity is 99.5% enters reactor A, is connect with catalyst A
Touch, generation includes the hydrocarbon mixture of low-carbon alkene and enters centrifugal station, isolates ethylene, propylene product, isolate C4~C6 hydrocarbon into
Enter reactor C, the hydrocarbon mixture of reactor C generations returns to centrifugal station, isolates more than C6 hydrocarbon and enters reactor B, reactor B life
Into hydrocarbon mixture return centrifugal station.Wherein, catalyst A be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 30, hydrogen
Shift index is 0.3, catalyst B be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 10, and catalyst C is ZSM-5 points
Sub- sieve catalyst, SiO2/Al2O3Molar ratio is 11, and reactor A is fixed bed, and reactor B is fixed bed, and reactor C is fluidisation
Bed, alkene mass percentage is 50% in C4~C6 hydrocarbon, and centrifugal station isolates low-carbon alkanes as product, in reactor A instead
The condition is answered to be：Reaction temperature is 400 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 5 seconds；Reactor C
Middle reaction condition is：Reaction temperature is 550 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 10 seconds；Instead
The reaction condition in device B is answered to be：Reaction temperature is 500 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 8
Second, the carbon-based selective mass fraction of reactor A outlet low-carbon alkene one way is 50%, and quality is added in reactor C chargings
Score is 1% vapor, and the vapor that mass fraction is 1% is added in reactor B charging.Product gas uses online gas phase color
Spectrum analysis, low-carbon alkene carbon base absorption rate are 62.98% weight.
【Embodiment 2】
According to condition described in embodiment 1 and step, catalyst A is ZSM-5 molecular sieve catalyst, SiO2/Al2O3Mole
Than being 200, hydrogen transfer index 0.21, catalyst B be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 80, catalysis
Agent C be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 100, and reactor A is moving bed, and reactor B is moving bed,
Reactor C is fluid bed, and alkene mass percentage is 62% in C4~C6 hydrocarbon, centrifugal station isolate low-carbon alkanes (ethane,
Propane and butane) as steam crack material, it is calculated according to yield of light olefins 50%, reaction condition is in reactor A：Reaction
Temperature is 550 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 1 second；Reaction condition is in reactor C：
Reaction temperature is 700 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 2 seconds；Reaction condition in reactor B
For：Reaction temperature is 650 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 1 second, and the reactor A goes out
The carbon-based selective mass fraction of mouth low-carbon alkene one way is 57%, and the water steaming that mass fraction is 50% is added in reactor C chargings
Gas adds the vapor that mass fraction is 50% in reactor B charging.Product gas uses online gas chromatographic analysis, low-carbon alkene
Hydrocarbon carbon base absorption rate is 70.34% weight.
【Embodiment 3】
According to condition described in embodiment 1 and step, catalyst A is ZSM-5 molecular sieve catalyst, SiO2/Al2O3Mole
Than being 80, hydrogen transfer index 0.17, catalyst B be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 50, catalyst
C be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 70, and reactor A is fluid bed, and reactor B is fluid bed, reaction
Device C is fluid bed, and alkene mass percentage is 71% in C4~C6 hydrocarbon, and centrifugal station isolates low-carbon alkanes (ethane, propane
And butane) as steam crack material, it is calculated according to yield of light olefins 50%, reaction condition is in reactor A：Reaction temperature
It it is 500 DEG C, reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 3 seconds；Reaction condition is in reactor C：Reaction
Temperature is 670 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 5 seconds；Reaction condition is in reactor B：
Reaction temperature is 620 DEG C, and reaction pressure is calculated as 0.01MPa with gauge pressure, and the gas phase residence time is 3 seconds, and the reactor A outlet is low
The carbon-based selective mass fraction of carbon olefin one way is 63%, the vapor that mass fraction is 20% is added in reactor C chargings, instead
Device B is answered to add the vapor that mass fraction is 10% in feeding.Product gas uses online gas chromatographic analysis, low-carbon alkene carbon
Base yield is 73.38% weight.
【Embodiment 4】
According to condition described in embodiment 1 and step, catalyst A is ZSM-5 molecular sieve catalyst, SiO2/Al2O3Mole
Than being 80, hydrogen transfer index 0.24, catalyst B be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 50, catalyst
C be ZSM-5 molecular sieve catalyst, SiO2/Al2O3Molar ratio is 70, and reactor A is fluid bed, and reactor B is fluid bed, reaction
Device C is fluid bed, and alkene mass percentage is 68% in C4~C6 hydrocarbon, and centrifugal station isolates low-carbon alkanes (ethane, propane
And butane) as steam crack material, it is calculated according to yield of light olefins 50%, reaction condition is in reactor A：Reaction temperature
It it is 510 DEG C, reaction pressure is calculated as 0.3MPa with gauge pressure, and the gas phase residence time is 4 seconds；Reaction condition is in reactor C：Reaction temperature
It is 680 DEG C to spend, and reaction pressure is calculated as 0.3MPa with gauge pressure, and the gas phase residence time is 5 seconds；Reaction condition is in reactor B：Reaction
Temperature is 625 DEG C, and reaction pressure is calculated as 0.3MPa with gauge pressure, and the gas phase residence time is 3 seconds, and the reactor A exports low-carbon alkene
The carbon-based selective mass fraction of hydrocarbon one way is 61%, and the vapor that mass fraction is 20%, reactor are added in reactor C chargings
The vapor that mass fraction is 10% is added in B chargings.Product gas uses online gas chromatographic analysis, the carbon-based receipts of low-carbon alkene
Rate is 72.55% weight.
【Comparative example 1】
According to condition described in embodiment 3 and step, reactor C is only not provided with, low-carbon alkene carbon base absorption rate is
68.22% weight.
【Comparative example 2】
According to condition described in embodiment 3 and step, reactor B is only not provided with, low-carbon alkene carbon base absorption rate is
69.37% weight.
Obviously, method using the present invention can achieve the purpose that improve yield of light olefins, excellent with larger technology
Gesture, available in the industrial production of low-carbon alkene.
Claims (3)
1. a kind of method by preparing low-carbon olefin by using methanol mainly includes the following steps that：
(1) it is mainly that the raw material of methanol enters reactor A, is contacted with catalyst A, generation includes the hydrocarbon mixture entrance of low-carbon alkene
Centrifugal station；The low-carbon alkene, i.e. ethylene and propylene；
(2) ethylene, propylene are isolated as product, C4~C6 hydrocarbon is isolated and enters reactor C and contacted with catalyst C, reactor C
The hydrocarbon mixture of generation returns to the centrifugal station, isolates more than C6 hydrocarbon and enters reactor B and is contacted with catalyst B, and reactor B is given birth to
Into hydrocarbon mixture return to the centrifugal station；
The catalyst A includes ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio is 30~200, and hydrogen transfer index is less than 0.3；It urges
Agent B includes ZSM-5 molecular sieve, SiO2/Al2O3Molar ratio is 10~80；Catalyst C includes ZSM-5 molecular sieve, SiO2/Al2O3
Molar ratio is 10~100；
The reactor A is fixed bed, moving bed or fluid bed；Reactor B is fixed bed, moving bed or fluid bed；Reactor C
For fluid bed；
Reaction condition is in reactor A：Reaction temperature is 400~550 DEG C, and reaction pressure is calculated as 0.01~0.3MPa with gauge pressure,
The gas phase residence time is 1~5 second；Reaction condition is in reactor C：Reaction temperature is 670~700 DEG C, and reaction pressure is with gauge pressure
0.01~0.3MPa is calculated as, the gas phase residence time is 2~10 seconds；Reaction condition is in reactor B：Reaction temperature is 500~620
DEG C, reaction pressure is calculated as 0.01~0.3MPa with gauge pressure, and the gas phase residence time is 1~8 second；
Alkene mass percentage is more than 50% in C4~C6 hydrocarbon；
The centrifugal station isolates low-carbon alkanes as product or as steam crack material.
2. according to claim 1 by the method for preparing low-carbon olefin by using methanol, it is characterised in that the reactor A exports low-carbon
The carbon-based selective mass fraction of alkene one way is more than 50%.
3. according to claim 1 by the method for preparing low-carbon olefin by using methanol, it is characterised in that in the reactor B, C chargings
The vapor that addition mass fraction is 1~50%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101165017A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Production increasing method for propylene |
| CN102464522A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Method for producing low-carbon olefins |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100632571B1 (en) * | 2005-10-07 | 2006-10-09 | 에스케이 주식회사 | Process for the preparation of light olefins in catalytic cracking from hydrocarbon feedstock |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101165017A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Production increasing method for propylene |
| CN102464522A (en) * | 2010-11-17 | 2012-05-23 | 中国石油化工股份有限公司 | Method for producing low-carbon olefins |
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