CN102649668A - Method for preparing ethylene from ethanol - Google Patents
Method for preparing ethylene from ethanol Download PDFInfo
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- CN102649668A CN102649668A CN2011100455713A CN201110045571A CN102649668A CN 102649668 A CN102649668 A CN 102649668A CN 2011100455713 A CN2011100455713 A CN 2011100455713A CN 201110045571 A CN201110045571 A CN 201110045571A CN 102649668 A CN102649668 A CN 102649668A
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- fluidized
- bed reactor
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Abstract
The invention relates to a method for preparing ethylene from ethanol, and mainly solves the technical problem of low reaction space velocity and low ethylene selectivity during the ethanol dehydration reaction process in the prior art. Through the adoption of the technical scheme that ethanol is taken as a raw material, and at least one of water and C2 to C5 alcohols is taken as a termination agent, and the method comprises the following steps: (a) the raw material enters from the bottom of a fluidized bed reactor at first, and is in contact reaction with catalysts in a dense zone and a transition zone in the reactor to generate an effluent I containing ethylene, propylene and the hydrocarbon catalyst; (b) the effluent I is in contact with the termination agent at the bottom of a gas-solid fast separation zone of the reactor to form an effluent II, and the effluent II enters into the gas-solid fast separation zone at the upper part of the fluidized bed reactor for gas-solid separation, gas enters into a follow-up working section for separation, and a solid catalyst enters into a regenerator for regeneration; and (c), the catalyst after regeneration returns to the reactor to continuously react. Therefore, the invention solves the problems well, and can be used in the industrial production of preparing ethylene from ethanol.
Description
Technical field
The present invention relates to a kind of method of producing ethylene with ethyl alcohol, particularly about adopting ethanol to transform the method for producing ethene through the fluidized-bed reactor efficient catalytic.
Background technology
Ethene is a kind of very important basic Organic Chemicals, and ethylene industry is the basis of petrochemical industry, in national economy, occupies very consequence.In recent years, along with increasing rapidly of verivate demands such as Vilaterm, the demand of ethene was all increased year by year.At present, ethene is raw material through Sweet natural gas or low-density oil cut mainly, adopts steam cracking process to make, but along with Sweet natural gas and low-density oil cut price continue highly, the method for some other approach increasing output of ethylene becomes the focus of concern.Especially along with the fast development of biotechnology, biological legal system alcoholic acid technology is constantly perfect, and the source of raw material is extensive day by day, and the cost of raw material also more becomes rationally, makes the producing ethylene from dehydration of ethanol technology enjoy attention.The producing ethylene from dehydration of ethanol technology has that flow process is short, equipment is few, investment is little, instant effect and characteristics such as stronger supporting flexibility and market handiness.Producing ethylene from dehydration of ethanol technology involved in the present invention is a kind of competitive Technology.
The main reaction of producing ethylene from dehydration of ethanol is:
CH
3CH
2OH→CH
2＝CH
2+H
2O
Be that the reaction of a part alcohol catalysis obtains a part ethene and a part water.Some side reactions also unavoidably can take place in the catalytic dehydration of ethanol process certainly as generating ether, acetaldehyde, carbon monoxide, carbonic acid gas, higher olefins etc.
1993 the 1st phases of document " Speciality Petrochemicals ", introduced a kind of employing for 35～37 pages
Sieve catalyst is to the research of low-concentration ethanol system ethene, and the result shows, when temperature of reaction is that 250～280 ℃, liquid air speed are 0.5～0.8 hour
-1, when the feed ethanol mass concentration was 10% left and right sides, ethanol conversion was up to 99%.But the catalyst liquid air speed is lower.
USP423475 has reported the producing ethylene from dehydration of ethanol technology, and it adopts oxide catalyst, 320～450 ℃ of temperature of reaction, and air speed 0.4～0.6 hour
-1The ethanol conversion that realizes under the condition.
Document CN200710034637.2 has introduced a kind of ZSM-5 catalyzer that is used for the producing ethylene from dehydration of ethanol reaction process, but the ethylene selectivity of this catalyzer is about 90%, and reaction preference is on the low side.
The subject matter that the related technology of above-mentioned document exists is to exist catalyzer and reaction product long invalid duration of contact, can not in time separate or stopped reaction, causes secondary reaction to take place easily; Side reaction is many; Amount of by-products is big, and is also lower with hourly space velocity, makes the low problem of purpose selectivity of product.
Summary of the invention
Technical problem to be solved by this invention is to exist in the producing ethylene by ethanol dehydration process in the technical literature in the past, and reaction velocity is low, and the problem that purpose product ethylene selectivity is low provides a kind of method of new producing ethylene with ethyl alcohol.The method of this producing ethylene with ethyl alcohol has the air speed height, the good advantage of purpose product ethylene selectivity.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopts is following: a kind of method of producing ethylene with ethyl alcohol is a raw material with ethanol, to be selected from water, C
2～C
5At least a in the alcohol is terminator, may further comprise the steps:
(a) raw material at first gets into from the fluidized-bed reactor bottom, in fluidized-bed reactor emulsion zone and zone of transition and catalyzer contact reacts, forms the elute I that contains ethene and catalyzer;
(b) the elute I from (a) step contacts with terminator in the bottom, gas-solid sharp separation district on fluidized-bed reactor zone of transition top; Form elute II; Elute II gets into the gas-solid sharp separation district on fluidized-bed reactor top after gas solid separation; Gas gets into follow-up workshop section to be separated, and solid catalyst gets into revivifier regeneration;
(c) return the fluidized-bed reactor bottom dense from the regenerated catalyst of revivifier and proceed reaction.
In the technique scheme in the fluidized-bed reactor zone of transition of emulsion zone through the undergauge structure link to each other with gas-solid sharp separation district.The reaction conditions of fluidized-bed reactor is preferably: temperature of reaction is 200～400 ℃, and reaction pressure is 0.01～1.5MPa, and be 0.1～20 second duration of contact, and catalyzer is 0.1～50 with the raw material weight ratio.The reaction conditions of fluidized-bed reactor is more preferably: temperature of reaction is 200～350 ℃, and reaction pressure is 0.05～1.0MPa, and be 0.2～10 second duration of contact, and catalyzer is 0.2～10 with the raw material weight ratio.The catalyzer preferred version is selected from least a or its composite molecular screen in ZSM-5, ZSM-11, ZSM-22, ZSM-35 or the ZSM-48 molecular sieve.Catalyzer more preferably scheme is selected from the ZSM-5 molecular sieve.The fluidized-bed reactor preferred version is selected from bubbling fluidized bed, turbulent fluidized bed, fast fluidized bed or riser reactor.Fluidized-bed reactor more preferably scheme is selected from fast fluidized bed.The weight ratio of raw material and terminator is 5～1000: 1, and the terminator feeding temperature is 10～200 ℃.
Adopt the ethanol dehydration alcohol catalysis to transform and produce in the ethylene process, purpose product ethene with catalyzer Long contact time situation under, still can continue to transform; When especially adopting ethanol dehydration fluidized bed reactor drum, at the settling zone of fluidized-bed reactor, a large amount of unsegregated catalyzer can continue under the condition of high temperature and reaction product generation secondary reaction; Make side reaction many; Amount of by-products is big, causes ethylene selectivity low, and yield is low.The present invention injects terminator through the zone, outlet position of leaving catalytic bed in catalyzer and reaction product; On the one hand; The terminator that temperature is lower contacts with pyroreaction mixture and catalyzer, can significantly reduce the temperature of reaction mixture and catalyzer, and this can further quicken the rapid temperature-fall period of pyroreaction mixture and catalyzer; After reaction mixture that temperature sharply reduces and catalyzer leave reaction zone; Side reaction is few, and the secondary reaction odds is little, has further improved the yield and the selectivity of purpose product.In addition, adopt fluidized-bed reactor, can make the temperature distribution of reaction bed more even, thereby the catalytic efficiency (of catalyzer is improved greatly, thereby reaction velocity is high.
The fluidized-bed reactor of producing ethylene with ethyl alcohol of the present invention is used for alcohol catalysis and transforms the production ethylene reaction, uses device shown in Figure 1, and adopting the ZSM-5 molecular sieve is catalyzer; Water is terminator, 200～400 ℃ of temperature of reaction, and 1～50 second duration of contact; Catalyzer and ethanol weight ratio are under 0.3～5 the condition; Ethanol conversion can reach 100%, and selectivity of ethylene can obtain better technical effect greater than 97%.
Description of drawings
Fig. 1 is fluidized-bed reactor synoptic diagram in the method for producing ethylene with ethyl alcohol of the present invention.
A is that emulsion zone, B are that zone of transition, C are negative areas, the 1st among Fig. 1, material inlet, the 2nd, sparger or grid distributor, the 3rd, interchanger, the 4th, riser tube; The 5th, settling vessel, the 6th, divide device soon, the 7th, gas tube, the 8th, cyclonic separator; The 9th, collection chamber, the outlet of 10 product gas, the 11st, stripper, the 12nd, regenerator sloped tube; The 13rd, inclined tube to be generated, the 14th, stripped vapor inlet, the 15th, terminator inlet.
Raw material is introduced by material inlet 1 among Fig. 1, and through gas distributor or grid distributor 2 laggard emulsion zone A and the catalyzer contact reacts of going into fluidized-bed that distribute, catalyzer and reaction mixture are through zone of transition B entering riser tube 4; Behind vortex quick separation device 6 sharp separation of riser tube 4 upper ends (end); Most of catalyzer gets into the lower region of settling vessel C; The part catalyzer that reaction mixture is carried secretly gets into settling vessel 5 top dilute phase spaces and carries out secondary separation through cyclonic separator 8; Product gas after the separation gets into collection chamber 9 through the outlet of cyclonic separator 8, is drawn by product gas outlet 10.Return the lower region of settling vessel 5 through the dipleg of cyclonic separator 8 from the catalyzer after cyclonic separator 8 separation.The reclaimable catalyst of the C bottom, negative area in the settling vessel 5 gets into stripper 11; Behind stripped vapor stripping from stripped vapor inlet 14; Get into revivifier (revivifier omits among the figure) through inclined tube 12 to be generated, regenerator gets into fluidized-bed reactor emulsion zone A through regenerator sloped tube 12.In addition, the part catalyzer in the settling vessel 5 continues reaction through the laggard fluidized-bed reactor emulsion zone A of going into of interchanger 3 heat exchange bottom with catalyst mix, and whole process circulation is carried out.
Through embodiment the present invention is done further elaboration below, but be not limited only to present embodiment.
Embodiment
[embodiment 1]
Accompanying drawing 1 shown device is adopted in test, is catalyzer with SAPO-34, and ethanol is raw material; Water is terminator, and the weight ratio of raw material and terminator is 20: 1, and the terminator feeding temperature is 30 ℃; The position that terminator injects is 1/6 of a riser tube height for the height apart from bottom, gas-solid sharp separation district, and the fluidized-bed reactor reaction conditions is: 350 ℃ of temperature of reaction, reaction pressure 0.05MPa; 7 seconds duration of contact, catalyzer and ethanol weight ratio are 1.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 96.7%.
[embodiment 2]
Accompanying drawing 1 shown device is adopted in test, with silica alumina ratio SiO
2/ Al
2O
3Be that 100 ZSM-5 is a catalyzer, ethanol is raw material, and water is terminator; The weight ratio of raw material and terminator is 5: 1, and the terminator feeding temperature is 80 ℃, and the position that terminator injects is 1/8 of a riser tube height for the height apart from bottom, gas-solid sharp separation district; The fluidized-bed reactor reaction conditions is: 320 ℃ of temperature of reaction; Reaction pressure 0.01MPa, 3 seconds duration of contact, catalyzer and ethanol weight ratio are 0.7.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 98.1%.
[embodiment 3]
Accompanying drawing 1 shown device is adopted in test, with silica alumina ratio SiO
2/ Al
2O
3Be that 60 ZSM-5 is a catalyzer, ethanol is raw material, and butanols is a terminator; The weight ratio of raw material and terminator is 10: 1, and the terminator feeding temperature is 40 ℃, and the position that terminator injects is 1/10 of a riser tube height for the height apart from bottom, gas-solid sharp separation district; The fluidized-bed reactor reaction conditions is: 270 ℃ of temperature of reaction; Reaction pressure 0.8MPa, 10 seconds duration of contact, catalyzer and ethanol weight ratio are 1.2.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 98.3%.
[embodiment 4]
Accompanying drawing 1 shown device is adopted in test, with silica alumina ratio SiO
2/ Al
2O
3Be that 200 ZSM-5 is a catalyzer, ethanol is raw material, and water is terminator; The weight ratio of raw material and terminator is 40: 1, and the terminator feeding temperature is 20 ℃, and the position that terminator injects is 1/3 of a riser tube height for the height apart from bottom, gas-solid sharp separation district; The fluidized-bed reactor reaction conditions is: 250 ℃ of temperature of reaction; Reaction pressure 1.2MPa, 15 seconds duration of contact, catalyzer and ethanol weight ratio are 7.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 98.8%.
[embodiment 5]
Accompanying drawing 1 shown device is adopted in test, is catalyzer with ZSM-11, and ethanol is raw material; Wherein the weight ratio of methyl alcohol and dme is 1: 1, and ethanol is terminator, and the weight ratio of raw material and terminator is 150: 1; The terminator feeding temperature is 30 ℃; The position that terminator injects is 1/4 of a riser tube height for the height apart from bottom, gas-solid sharp separation district, and the fast fluidized bed reactor reaction conditions is: 220 ℃ of temperature of reaction, reaction pressure 0.2MPa; 5 seconds duration of contact, catalyzer and ethanol weight ratio are 0.5.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 98.1%.
[embodiment 6]
Accompanying drawing 1 shown device is adopted in test, is catalyzer with ZSM-35 and SAPO-34 composite molecular screen, and ZSM-5 accounts for 10% in the catalyzer; SAPO-34 accounts for 80%, and ethanol is raw material, and propyl alcohol is a terminator; The weight ratio of raw material and terminator is 5: 1, and the terminator feeding temperature is 50 ℃, and the position that terminator injects is 1/5 of a riser tube height for the height apart from bottom, gas-solid sharp separation district; The fluidized-bed reactor reaction conditions is: 230 ℃ of temperature of reaction; Reaction pressure 0.2MPa, 8 seconds duration of contact, catalyzer and ethanol weight ratio are 1.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 97.3%.
[embodiment 7]
Accompanying drawing 1 shown device is adopted in test, is catalyzer with ZSM-22, and ethanol is raw material; Water is terminator, and the weight ratio of raw material and terminator is 80: 1, and the terminator feeding temperature is 30 ℃; The position that terminator injects is 1/10 of a riser tube height for the height apart from bottom, gas-solid sharp separation district, and the fluidized-bed reactor reaction conditions is: 210 ℃ of temperature of reaction, reaction pressure 0.4MPa; 5 seconds duration of contact, catalyzer and ethanol weight ratio are 3.Its reaction result is: ethanol conversion 98.7%, ethylene selectivity are 98.8%.
[embodiment 8]
Accompanying drawing 1 shown device is adopted in test, is catalyzer with ZSM-48, and ethanol is raw material; Water is terminator, and the weight ratio of raw material and terminator is 50: 1, and the terminator feeding temperature is 30 ℃; The position that terminator injects is 1/6 of a riser tube height for the height apart from bottom, gas-solid sharp separation district, and the riser reactor reaction conditions is: 250 ℃ of temperature of reaction, reaction pressure 0.1MPa; 3 seconds duration of contact, catalyzer and ethanol weight ratio are 0.3.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 98.5%.
[embodiment 9]
Accompanying drawing 1 shown device is adopted in test, is catalyzer with ZSM-35, and ethanol is raw material; Water is terminator, and the weight ratio of raw material and terminator is 40: 1, and the terminator feeding temperature is 100 ℃; The position that terminator injects is 1/8 of a riser tube height for the height apart from bottom, gas-solid sharp separation district, and the fluidized-bed reactor reaction conditions is: 250 ℃ of temperature of reaction, reaction pressure 0.1MPa; 3 seconds duration of contact, catalyzer and ethanol weight ratio are 3.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 98.3%.
[comparative example 1]
Accompanying drawing 1 shown device is adopted in test, according to condition and the catalyzer of embodiment 1, does not just add terminator in the device.Its reaction result is: ethanol conversion 100%, ethylene selectivity are 95.1%.
[comparative example 2]
Fixed-bed reactor are adopted in test, and condition and catalyzer according to embodiment 8 do not add terminator, and its reaction result is: ethanol conversion 95%, ethylene selectivity are 93.5%.
Claims (9)
1. the method for a producing ethylene with ethyl alcohol is a raw material with ethanol, to be selected from water, C
2～C
5At least a in the alcohol is terminator, may further comprise the steps:
(a) raw material at first gets into from the fluidized-bed reactor bottom, in fluidized-bed reactor emulsion zone and zone of transition and catalyzer contact reacts, forms the elute I that contains ethene and catalyzer;
(b) the elute I from (a) step contacts with terminator in the bottom, gas-solid sharp separation district on fluidized-bed reactor zone of transition top; Form elute II; Elute II gets into the gas-solid sharp separation district on fluidized-bed reactor top after gas solid separation; Gas gets into follow-up workshop section to be separated, and solid catalyst gets into revivifier regeneration;
(c) return the fluidized-bed reactor bottom dense from the regenerated catalyst of revivifier and proceed reaction.
2. according to the method for the said producing ethylene with ethyl alcohol of claim 1, it is characterized in that emulsion zone in the fluidized-bed reactor links to each other with gas-solid sharp separation district through the zone of transition of undergauge structure.
3. according to the method for the said producing ethylene with ethyl alcohol of claim 1, the temperature of reaction that it is characterized in that fluidized-bed reactor is 200～400 ℃, and reaction pressure is 0.01～1.5MPa, and be 0.1～20 second duration of contact, and catalyzer is 0.1～50 with the raw material weight ratio.
4. according to the method for the said producing ethylene with ethyl alcohol of claim 3, it is characterized in that the fluidized-bed reactor temperature of reaction is 200～350 ℃, reaction pressure is 0.05～1.0MPa, and be 0.2～10 second duration of contact, and catalyzer is 0.2～10 with the raw material weight ratio.
5. according to the method for the said producing ethylene with ethyl alcohol of claim 1, it is characterized in that catalyzer is selected from least a or its composite molecular screen in SAPO-34, ZSM-5, ZSM-11, ZSM-22, ZSM-35 or the ZSM-48 molecular sieve.
6. according to the method for the said producing ethylene with ethyl alcohol of claim 5, it is characterized in that catalyzer is selected from the ZSM-5 molecular sieve.
7. according to the method for the said producing ethylene with ethyl alcohol of claim 1, it is characterized in that fluidized-bed reactor is selected from bubbling fluidized bed, turbulent fluidized bed, fast fluidized bed or riser reactor.
8. according to the method for the said producing ethylene with ethyl alcohol of claim 7, it is characterized in that fluidized-bed reactor is selected from fast fluidized bed.
9. according to the method for the said producing ethylene with ethyl alcohol of claim 1, the weight ratio that it is characterized in that raw material and terminator is 5～1000: 1, and the terminator feeding temperature is 10～100 ℃.
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| CN2011100455713A CN102649668A (en) | 2011-02-25 | 2011-02-25 | Method for preparing ethylene from ethanol |
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| CN2011100455713A CN102649668A (en) | 2011-02-25 | 2011-02-25 | Method for preparing ethylene from ethanol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108101727A (en) * | 2018-01-12 | 2018-06-01 | 温州市星峰新材料有限公司 | A kind of method of producing ethylene from dehydration of ethanol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101165027A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from oxygen-containing compounds |
| CN101164684A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Combined fluidized bed reactor |
| CN101306969A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Reaction device for preparing low-carbon olefin from oxygen-containing compounds |
-
2011
- 2011-02-25 CN CN2011100455713A patent/CN102649668A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101165027A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Method for producing ethylene and propylene from oxygen-containing compounds |
| CN101164684A (en) * | 2006-10-20 | 2008-04-23 | 中国石油化工股份有限公司 | Combined fluidized bed reactor |
| CN101306969A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Reaction device for preparing low-carbon olefin from oxygen-containing compounds |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108101727A (en) * | 2018-01-12 | 2018-06-01 | 温州市星峰新材料有限公司 | A kind of method of producing ethylene from dehydration of ethanol |
| CN108101727B (en) * | 2018-01-12 | 2020-11-03 | 温州市星峰新材料有限公司 | Method for preparing ethylene by ethanol dehydration |
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Application publication date: 20120829 |