CN102372566A - Method for preparing ethene through ethanol dehydration - Google Patents
Method for preparing ethene through ethanol dehydration Download PDFInfo
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- CN102372566A CN102372566A CN2010102608047A CN201010260804A CN102372566A CN 102372566 A CN102372566 A CN 102372566A CN 2010102608047 A CN2010102608047 A CN 2010102608047A CN 201010260804 A CN201010260804 A CN 201010260804A CN 102372566 A CN102372566 A CN 102372566A
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Abstract
The invention relates to a method for preparing ethene through ethanol dehydration, and mainly aims to solve the problem of small production capacity of a single reactor in previous methods of ethene preparation through ethanol dehydration. The invention adopts a mode of molten salt external circulation. Specifically, annular molten salt channels are arranged at two ends of a reactor housing, holes are disposed at corresponding positions by which the upper and lower molten salt channel contact with the housing wall, the upper and lower molten salt channel are respectively provided with a molten salt inlet and a molten salt outlet, a baffle plate is installed inside the reactor housing, and the baffle plate is equipped with channels through which molten salt can flow. The method of the invention can be used in the industrial production of ethene through ethanol dehydration.
Description
Technical field
The present invention relates to a kind of method of producing ethylene from dehydration of ethanol.
Background technology
Ethene is crucial petrochemical materials, and its large derived product mainly contains Vilaterm, oxyethane, terepthaloyl moietie, SE, vinylbenzene, vinyl acetate between to for plastic etc.
In the process method of producing ethylene from dehydration of ethanol, in disclosed document or the patent many methods are arranged at home and abroad, its basic technology mainly is divided into fixed-bed process and fluidized-bed process.ABB Lummus company once proposes to carry out ethanol dehydration reaction with fluidization at late nineteen seventies and produces ethene (USP4134926), but this technology does not obtain industrial applications as yet.At present industrial application be mainly fixed-bed process, comprise isothermal fixed-bed process and insulation fix bed technology.
Initial ethanol dehydration reaction carries out in calandria type fixed bed, and reaction pressure is a normal pressure, adopts direct heating or utilizes the mode of heating medium (like fused salt) indirect heating for reaction reaction heat to be provided.But in the prior art, be that raw material carries out the calandria type fixed bed reactor device that biological ethane is produced with ethanol at home, adopt heating tube to be built in the reactor shell, pre-reactor is formed one, constitutes the structure formation of circulating inside.Reacting required heat is provided by fused salt indirectly, and reactor drum is advanced in the disposable filling of the fused salt of heat transfer usefulness, during the reaction needed heat; By the heating of the electrically heated rod in heating tube fused salt; Be the reaction heat supply, because the restriction of type of heating, there is following problem in this reactor drum: 1, the separate unit throughput of device is limited; The separate unit throughput of existing apparatus can't satisfy the demand of market development all less than 10,000 tons/year; 2, device uses time unit's output energy consumption big, and effective rate of utilization is low, and equipment running cost is high.
Summary of the invention
Technical problem to be solved by this invention is the fixed-bed reactor separate unit throughput problem of smaller of producing ethylene from dehydration of ethanol in the prior art, and a kind of method of new producing ethylene from dehydration of ethanol is provided.This method has that structure of reactor is reasonable, and heat supply is even, separate unit throughput big advantage.
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 from dehydration of ethanol is a raw material with ethanol, is 100～500 ℃ in temperature of reaction, and reaction pressure is 0.01～3.0MPa, and the liquid weight air speed is 0.1～8.0 hour
-1Condition under; Raw material generates ethene with the catalyzer contact reacts in reactor drum; Said reactor drum comprises reactor shell, upper cover, lower cover, upper tubesheet and lower tubesheet, and the top end of the upper and lower end socket of reactor drum is respectively equipped with material inlet and material outlet, is vertically installed with tubulation between the upper and lower tube sheet of reactor drum; Tubulation is connected with upper cover and lower cover respectively, is mounted with catalyzer in the tubulation; The two ends up and down in the reactor shell outside are respectively equipped with fused salt passage and following fused salt passage on the annular; On described upper and lower fused salt passage and corresponding site that housing wall contacts, offer at least 4 square holes respectively; On described upper and lower fused salt passage, be respectively equipped with the outlet of fused salt import and fused salt; Get in the square hole entering housing of fused salt through fused salt lower channel corresponding site of fused salt import; Get into the fused salt upper channel with the square hole through fused salt upper channel corresponding site after the tubulation heat exchange, discharge by the fused salt outlet.Wherein reactor shell inside is provided with the annular traverse baffle that at least one diameter equates with the housing internal diameter apart from the total strong point of the tubulation of upper tubesheet 1/10～9/10; Offer position and the tubulation corresponding pore of arranging on the traverse baffle; Pore diameter is greater than the tubulation external diameter, and tubulation vertically passes traverse baffle through the pore on the traverse baffle; In addition, have the aperture that can supply the fused salt circulation on the traverse baffle.
In technique scheme, preferably in reactor shell evenly, be symmetrical set traverse baffle.Preferred traverse baffle quantity is 3～5, promptly establishes upper and lower traverse baffle respectively apart from upper tubesheet 1/6～5/6 housing length overall place, traverse baffle in the middle of establishing between the traverse baffle up and down.The traverse baffle preferred version is an annular, is 1.1: 1～1.6: 1 with the arrange ratio preferable range of diameter and the external diameter of tubulation of the pore that is complementary of tubulation on the traverse baffle.Can supply the aperture perforated area that fused salt passes through and the ratio of reactor cross-sectional area on the traverse baffle is 1: 40～1: 20; The perforate rule of aperture is for to reduce in the aperture along the reactor drum radial direction from inside to outside successively.Described going up on fused salt passage and the corresponding site that housing wall contacts offers at least 4 square holes; The perforate rule is for being reduced to the two side holes height by fused salt outlet successively, and the perforate rule on described fused salt passage down and the corresponding site that housing wall contacts is for to be increased to the two side holes height by the fused salt import successively.The ratio of the area of the corresponding site that the perforated area on the housing wall in the upper and lower fused salt passage and fused salt passage contact with housing wall is 1: 8～1: 2.Fused salt import and exit preferred version are circular array for being provided with two curved baffles.The catalyzer preferred version is an aluminum oxide.Tubulation radical preferable range is at least 100.
The present invention is provided with the fused salt passage on reactor shell, and the perforate on the housing wall in the fused salt passage, guarantees that fused salt equivalent enters in the reactor shell, thereby solves the uneven problem of temperature distribution in the reactor shell.Traverse baffle is set in reactor shell, and its effect mainly is enhance fluid mobile turbulent extent between pipe, enhancing heat transfer; Improve heat transfer efficiency, so in theory, traverse baffle quantity is many more; The fused salt heat-transfer effect is good more, and still along with the increase of traverse baffle quantity, the manufacturing cost of reactor drum and manufacture difficulty can significantly increase; So, comprehensive cost and manufacturing factor, the traverse baffle quantity among the present invention in the reactor drum is controlled at 10 with interior relatively good.Because traverse baffle central position fused salt speed of circulation is slow, it is inhomogeneous to conduct heat, and temperature distribution is also inhomogeneous; Therefore be provided with circular perhaps polygonal hole through the traverse baffle center and realize not stringing of this zone; Not only be provided with the pore that matees with tubulation on the traverse baffle, also be provided with the aperture that can supply fused salt to pass through, make fused salt add the cross-flow mode for advection in the intravital motion of reactor enclosure; With cross-flow is main, and advection is auxilliary.Through above setting make fused salt can be evenly, fast at the reactor drum internal recycle, the heat that postreaction timely is required, guarantee fused salt axially, radial temperature difference can remain in the scope of permission.Reactor drum of the present invention adopts the fused salt external circulation mode; Fused salt is after the reactor enclosure external is heated; Entering in the reactor shell provides heat, this method not to receive the restriction of electrically heated rod heating power for reacting, and reactor diameter can reach 3～4 meters; Thereby the throughput of separate unit reactor drum is improved greatly, obtained better technical effect.
Description of drawings
Fig. 1 is a producing ethylene from dehydration of ethanol reactor drum synoptic diagram of the present invention.
Fig. 2 is fused salt flow schematic diagram in the upper channel xsect of reactor drum of the present invention.
Fig. 3 is fused salt flow schematic diagram in the lower passage xsect of reactor drum of the present invention.
Fig. 4 is provided with synoptic diagram for the fused salt passage on the traverse baffle of reactor drum of the present invention.
Fig. 5 is the stretch-out view at center with fused salt ingress for perforate rule on the lower passage inner housing of reactor drum of the present invention.
Fig. 6 is the stretch-out view at center with the fused salt exit for perforate rule on the upper channel inner housing of reactor drum of the present invention.
Shown in figure: 1 is material inlet, and 2 is the reactor drum end socket, and 3 is the reactor drum upper tubesheet, and 4 is the fused salt upper channel; 5 are the fused salt outlet, and 6 is reactor shell, and 7 is traverse baffle, and 8 is the fused salt import; 9 is the reactor drum tubulation, and 10 is the fused salt lower channel, and 11 is material outlet, and 12 is baffle plate; 13 is the annular space hole, and 14 is aperture, and 15 are the fused salt flow direction.
When the reactor drum that method of the present invention adopted was worked, reactant gases carried out dehydration reaction from the tubulation 9 that material inlet 1 gets in the reactor shell 6, and discharges the entering next process through material outlet 11.In reaction; Open pump for liquid salts; Make fused salt pass through fused salt import 8 and get into fused salt lower channel 9; The hole of not waiting through size on the reactor shell then gets in the reactor shell 6, and fused salt through being that master, cross-flow are that the mode of assisting circulates with the advection, provides reaction required heat in reactor shell 6.Behind the fused salt inflow reactor housing 6; In the middle of flowing to uniformly earlier, behind traverse baffle 7, begin the advection mode again and upwards flow; Flow through annular space hole 13 and aperture 14 on the traverse baffle; The hole of not waiting through the size on the reactor shell then gets into fused salt upper channel 4, gets into Salt heater through fused salt outlet 5, gets into reactor drum after the supplementing energy once more.
Through embodiment the present invention is done further elaboration below.
Embodiment
[embodiment 1]
The ethanol of 95 volume % is 350 ℃ in temperature of reaction, and reaction pressure is 0.04MPaG, and the liquid volume space velocity of ethanol is that dehydration generates ethene under the effect of aluminium oxide catalyst under 0.8 hour-1 the condition, and the reaction employing is like the reactor drum of Fig. 1.The reactor drum scale is 20000 tons of/year ethene, several 1142 of reactor drum tubulation, 2.2 meters of reactor body diameters.The two ends up and down of columnar reactor shell 6 are provided with material inlet 1 and material outlet 10; The two ends up and down of reactor shell 6 are provided with fused salt upper channel 4 and fused salt lower channel 10; And be provided with fused salt outlet 5 and fused salt import 8; 1/4 place and 3/4 place apart from upper tubesheet in the reactor shell 6 are provided with circular last traverse baffle and following traverse baffle respectively; 1/2 place apart from upper tubesheet is provided with circular middle traverse baffle, and the little hole area that can supply fused salt to pass through on the traverse baffle plate is 1: 40 with the long-pending ratio of reactor shell inner section; The housing that fused salt import 8 and fused salt export 5 places is provided with the baffle plate 12 of circular arc.The ratio of the area of the corresponding site that the square hole perforated area on the reactor enclosure body wall at fused salt upper channel 4 and fused salt lower channel 10 places and fused salt passage contact with housing wall is 1: 5, and axial temperature difference is 5～10 ℃ in the reactor shell, and radial temperature difference is 3～5 ℃.
[embodiment 2]
Reaction conditions is with embodiment 1; The reactor drum scale is with embodiment 1; Other geometrical dimensions of reactor drum are with embodiment 1; Just 1/6 place, 1/3 place, 2/3 place and 5/6 place apart from upper tubesheet is provided with circular last traverse baffle and following traverse baffle respectively in the reactor shell 6, is provided with the middle traverse baffle of circle apart from 1/2 place of upper tubesheet, and the little hole area that can supply fused salt to pass through on the traverse baffle plate is 1: 20 with the long-pending ratio of reactor shell inner section; The ratio of the area of the corresponding site that the square hole perforated area on the reactor enclosure body wall at fused salt upper channel 4 and fused salt lower channel 10 places and fused salt passage contact with housing wall is 1: 8, and axial temperature difference is 5～10 ℃ in the reactor shell, and radial temperature difference is 2～8 ℃.
[embodiment 3]
Reaction conditions is with embodiment 1; The reactor drum scale is with embodiment 1; Other geometrical dimensions of reactor drum are with embodiment 1; Just 1/3 place and 2/3 place apart from upper tubesheet is provided with circular last traverse baffle and following traverse baffle respectively in the reactor shell 6, and the little hole area that can supply fused salt to pass through on the traverse baffle plate is 1: 30 with the long-pending ratio of reactor shell inner section; The ratio of the area of the corresponding site that the square hole perforated area on the reactor enclosure body wall at fused salt upper channel 4 and fused salt lower channel 10 places and fused salt passage contact with housing wall is 1: 2, and axial temperature difference is 5～10 ℃ in the reactor shell, and radial temperature difference is 3～8 ℃.
[embodiment 4]
Reaction conditions is with embodiment 1, and the reactor drum scale is 10000 tons of/year ethene, several 572 of reactor drum tubulation, 1.6 meters of reactor body diameters.Other geometrical dimensions of reactor drum just evenly are provided with 7 traverse baffles in the reactor shell 6 with embodiment 1, and the little hole area that can supply fused salt to pass through on the traverse baffle is 1: 25 with the long-pending ratio of reactor shell inner section; The ratio of the area of the corresponding site that the square hole perforated area on the reactor enclosure body wall at fused salt upper channel 4 and fused salt lower channel 10 places and fused salt passage contact with housing wall is 1: 4, and axial temperature difference is 5～10 ℃ in the reactor shell, and radial temperature difference is 2～5 ℃.
[embodiment 5]
The reactor drum specification is with embodiment 1, and the reactor drum scale is with embodiment 1, and temperature of reaction is 390 ℃, and other reaction conditionss are with embodiment 1, and axial temperature difference is 5～10 ℃ in the reactor shell, and radial temperature difference is 3～7 ℃.
[embodiment 6]
The reactor drum specification is with embodiment 1, and the reactor drum scale is with embodiment 1, and other reaction conditionss are with embodiment 1, and the liquid volume space velocity of ethanol is 2.0 hours
-1Condition under, axial temperature difference is 5～10 ℃ in the reactor shell, radial temperature difference is 3～8 ℃.
[comparative example]
Reaction conditions is with embodiment 1, and the reactor drum scale is with embodiment 4, and reactor drum adopts the shell-and-tube reactor of fused salt circulating inside, and axial temperature difference is 10～15 ℃ in the reactor shell, and radial direction temperature difference is 5～10 ℃.
Claims (10)
1. the method for a producing ethylene from dehydration of ethanol is a raw material with ethanol, is 100～500 ℃ in temperature of reaction, and reaction pressure is 0.01～3.0MPa, and the liquid weight air speed is 0.1～8.0 hour
-1Condition under; Raw material generates ethene with the catalyzer contact reacts in reactor drum; Said reactor drum comprises reactor shell, upper cover, lower cover, upper tubesheet and lower tubesheet, and the top end of the upper and lower end socket of reactor drum is respectively equipped with material inlet and material outlet, is vertically installed with tubulation between the upper and lower tube sheet of reactor drum; Tubulation is connected with upper cover and lower cover respectively, is mounted with catalyzer in the tubulation; The two ends up and down in the reactor shell outside are respectively equipped with fused salt passage and following fused salt passage on the annular; On described upper and lower fused salt passage and corresponding site that housing wall contacts, offer at least 4 square holes respectively; On described upper and lower fused salt passage, be respectively equipped with the outlet of fused salt import and fused salt; Get in the square hole entering housing of fused salt through fused salt lower channel corresponding site of fused salt import; Get into the fused salt upper channel with the square hole through fused salt upper channel corresponding site after the tubulation heat exchange, discharge by the fused salt outlet; Wherein reactor shell inside is provided with the annular traverse baffle that at least one diameter equates with the housing internal diameter apart from the total strong point of the tubulation of upper tubesheet 1/10～9/10; Offer position and the tubulation corresponding pore of arranging on the traverse baffle; Pore diameter is greater than the tubulation external diameter, and tubulation vertically passes traverse baffle through the pore on the traverse baffle; In addition, have the aperture that can supply the fused salt circulation on the traverse baffle.
2. the method for producing ethylene from dehydration of ethanol according to claim 1 is characterized in that the pore diameter and the ratio of tubulation external diameter are 1.1～1.6: 1.
3. the method for producing ethylene from dehydration of ethanol according to claim 1 is characterized in that the ratio of the area of the corresponding site that described square hole perforated area and fused salt passage contact with housing wall is 1: 8～1: 2; The perforate rule of fused salt upper channel reduces to the two side holes height for being exported by fused salt successively, and the perforate rule of fused salt lower channel is for to be increased to the two side holes height by the fused salt import successively.
4. the method for producing ethylene from dehydration of ethanol according to claim 1 is characterized in that traverse baffle is 2～7.
5. the method for producing ethylene from dehydration of ethanol according to claim 4 is characterized in that traverse baffle is 3～5.
6. the method for producing ethylene from dehydration of ethanol according to claim 1 is characterized in that traverse baffle is even, is symmetricly set in the reactor drum; Can supply the aperture perforated area that fused salt passes through and the ratio of reactor cross-sectional area on the traverse baffle is 1: 40～1: 20.
7. the method for producing ethylene from dehydration of ethanol according to claim 1, the perforate rule that it is characterized in that aperture on the traverse baffle is for to reduce in the aperture along the reactor drum radial direction from inside to outside successively.
8. the method for producing ethylene from dehydration of ethanol according to claim 1 is characterized in that fused salt import and exit are provided with two curved baffles, are circular array.
9. the method for producing ethylene from dehydration of ethanol according to claim 1 is characterized in that described catalyzer is an aluminum oxide.
10. the method for producing ethylene from dehydration of ethanol according to claim 1 is characterized in that the tubulation radical in the described reactor drum is at least 100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102608047A CN102372566A (en) | 2010-08-23 | 2010-08-23 | Method for preparing ethene through ethanol dehydration |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102608047A CN102372566A (en) | 2010-08-23 | 2010-08-23 | Method for preparing ethene through ethanol dehydration |
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| CN102372566A true CN102372566A (en) | 2012-03-14 |
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| CN2010102608047A Pending CN102372566A (en) | 2010-08-23 | 2010-08-23 | Method for preparing ethene through ethanol dehydration |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108371931A (en) * | 2017-12-29 | 2018-08-07 | 安丽华 | A kind of production equipment of synthesized micromolecule amount polyphenylene oxide |
| WO2019223033A1 (en) * | 2018-05-25 | 2019-11-28 | An Lihua | MULTIPHASE REACTOR FOR PREPARING ALDEHYDE USING α-ALKENE HYDROFORMYLATION REACTION AND PREPARATION METHOD |
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| US20040213711A1 (en) * | 2002-07-10 | 2004-10-28 | Kyoung-Su Ha | Catalytic oxidation reactor with enhanced heat exchanging system |
| CN201008786Y (en) * | 2006-10-11 | 2008-01-23 | 西安航天华威化工生物工程有限公司 | Fixed bed reactor for producing by benzene method capable of producing 20,000 tons per year |
| CN101172920A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for producing ethylene with ethanol dehydration |
| CN101768041A (en) * | 2009-01-07 | 2010-07-07 | 中国石油化工股份有限公司 | Method for preparing ethylene by dehydrating ethanol |
-
2010
- 2010-08-23 CN CN2010102608047A patent/CN102372566A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040213711A1 (en) * | 2002-07-10 | 2004-10-28 | Kyoung-Su Ha | Catalytic oxidation reactor with enhanced heat exchanging system |
| CN201008786Y (en) * | 2006-10-11 | 2008-01-23 | 西安航天华威化工生物工程有限公司 | Fixed bed reactor for producing by benzene method capable of producing 20,000 tons per year |
| CN101172920A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for producing ethylene with ethanol dehydration |
| CN101768041A (en) * | 2009-01-07 | 2010-07-07 | 中国石油化工股份有限公司 | Method for preparing ethylene by dehydrating ethanol |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108371931A (en) * | 2017-12-29 | 2018-08-07 | 安丽华 | A kind of production equipment of synthesized micromolecule amount polyphenylene oxide |
| CN108371931B (en) * | 2017-12-29 | 2020-07-03 | 上海载正化工科技发展有限公司 | Production equipment for synthesizing polyphenylene ether with small molecular weight |
| WO2019223033A1 (en) * | 2018-05-25 | 2019-11-28 | An Lihua | MULTIPHASE REACTOR FOR PREPARING ALDEHYDE USING α-ALKENE HYDROFORMYLATION REACTION AND PREPARATION METHOD |
| CN110523348A (en) * | 2018-05-25 | 2019-12-03 | 安丽华 | A kind of alpha-olefin hydroformylation reaction prepares the heterophase reactor and preparation method of aldehyde |
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Application publication date: 20120314 |