CN102372559A - Ethylene separation method - Google Patents
Ethylene separation method Download PDFInfo
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- CN102372559A CN102372559A CN2010102601870A CN201010260187A CN102372559A CN 102372559 A CN102372559 A CN 102372559A CN 2010102601870 A CN2010102601870 A CN 2010102601870A CN 201010260187 A CN201010260187 A CN 201010260187A CN 102372559 A CN102372559 A CN 102372559A
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Abstract
The invention relates to an ethylene separation method, which mainly solves the problems of large loss amount of ethylene in an ethylene rectifying tower and low recovery rate of ethylene in prior art. The separation method of the invention is characterized in that the crude ethylene is compressed and dried to enter in the ethylene rectifying tower, a material flow at the top of the ethylene rectifying tower enters into a light component eliminating tower for separating, a light component is eliminated at the top of the light component eliminating tower to obtain a ethylene product; a material in a tower kettle of the ethylene rectifying tower is flash evaporated through a flash evaporation pot, the material at the top enters in the bottom part of the ethylene rectifying tower, a part of the material at the bottom circularly enters in a central part of the flash evaporation pot, the other part of the material is discharged outside. The technical scheme better solves the problems and can be used in industrial production of ethylene.
Description
Technical field
The present invention relates to a kind of ethene separation method.
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.
The production technique of producing ethylene from dehydration of ethanol and the catalyzer of use thereof are all known.Main research direction is to improve technical process at present, reduces the ethanol unit consumption, increases the economic benefit of device.
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.In reaction process, temperature of reaction and material flow are key factors, if temperature is too high or material flow is too low, will cause the generation of by product; But along with the increase of flow velocity, ethanol conversion can descend again.In order to solve this contradiction; Brazil Petrobras company has proposed the adiabatic technology (USP4232179) of ethanol dehydration reaction; Be that ethanol dehydration reaction carries out in insulation fix bed, reaction mass is heated to reaction before getting into reactor drum temperature required, to guarantee normally carrying out of reaction.Afterwards, the said firm has proposed the insulation fix bed reaction process of syllogic again, and utilizes this technology to set up 60,000 tons of/year ethylene units of a cover in the early 1980s.Patent USP4396789 has disclosed some basic conditions of this technology: adopt three placed in-line insulation fix bed reactors; Come the ethanol and the steam charging of each Reactor inlet of preheating with a stove, by products such as unreacted ethanol and ether are carried out circulation.The adding of steam has reduced the reaction coking, has prolonged activity of such catalysts, has improved productive rate.400～520 ℃ of temperature of reaction, under the condition of reaction pressure 2.0～4.0MPaG, the ethanol conversion of separate unit reactor drum is greater than 96%, and the total ethanol transformation efficiency is near 100%.Nineteen seventies, Halcon company has developed the double mode reaction technology of a kind of trade mark for the silicon-Al catalysts and the thermal insulation/isothermal fixed bed of " Syndol ", and wherein the isothermal bed technology has obtained industrial applications.Reaction result shows: at 318 ℃ of temperature of reaction, liquid weight air speed (WLHSV) 0.23～0.40h
-1Condition under, ethylene selectivity reaches 96.8% (mol), ethanol conversion is 97～99%.After; Halcon/SD company has developed multistage insulation fixed bed reaction process again: ethanol gets into dehydration generation ethene in the multistage insulation fixed bed reaction in water vapor dilution back; Reactant gases carries out low temperature fractionation again after washing, compression, alkali cleaning and drying, obtain ethylene product at last.Testing data shows: at 335～450 ℃ of temperature of reaction, liquid weight air speed (WHSV) 0.79～1.17h
-1Condition under, ethylene selectivity reaches 95～98% (mol), ethanol conversion is 97～99%.
The high-temperature gas product that reactor is discharged gets into the washing system of being made up of water scrubber, compressor and caustic wash tower after cooling condensation reclaims heat, ethylene gas gets into water scrubber, compressor and caustic wash tower successively and washs; Ethylene gas after washing gets into drying system; Ethene after dry gets into the ethene treating column, separates light component, obtains ethylene product at the tower still.Typical process operational condition on the full scale plant is at present: the ethylene rectification tower tower top pressure is 2.65MPaG, and tower top temperature is-17 ℃, and tower still pressure is 2.69MPaG, and tower still temperature is-9 ℃, and reflux ratio is 2.7, and the phegma temperature is-20 ℃.Because the normal boiling point of ethene and ethane is very approaching, often has a certain amount of ethene at the bottom of the ethylene distillation Tata in the fraction.The ethylene recovery rate that ethylene rectification tower is gone up in industry at present is about 96%, and the ethene of carrying secretly in the still liquid is too much, causes the loss of ethene.Therefore, how to reduce that the loss of ethene is a good problem to study at the bottom of the ethylene distillation Tata.Owing to adopt flash tank that adiabatic flash is carried out in heavy constituent, reclaim the ethene in the still liquid to greatest extent among the present invention, to reduce the device material consumption.
Summary of the invention
Technical problem to be solved by this invention is to overcome in the prior art the more problem of ethylene loss in the ethene treating process, so that a kind of new ethene separation method to be provided.This method has that the ethylene loss amount is few, facility investment is low, the characteristics of easy handling.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following: a kind of ethene separation method may further comprise the steps: a) contain ethene, ethane and C
3And the mixture of above heavy constituent entering ethylene rectification tower middle and lower part, isolate the ethylene streams I that contains light constituent at cat head, the tower still is isolated and is mainly contained ethane, C
3And the heavy constituent logistics II of above component; B) the logistics II drains into the flash tank middle part; Behind the flash tank adiabatic flash; Flash drum overhead discharge contain a small amount of heavy constituent ethene to the ethylene rectification tower bottom, the heavy constituent part circulation that discharge the flash tank bottom gets into the flash tank middle part, another part is then discharged out-of-bounds; C) the logistics I gets into the lightness-removing column top, obtains containing the light constituent of hydrogen, methane and carbon monoxide at cat head, and the tower still obtains ethylene product.
In the technique scheme; The optimized technical scheme ethylene rectification tower adopts packing tower or tray column; The theoretical tray sum preferable range of ethylene rectification tower is 50～120, and wherein rectifying section theoretical plate number preferable range is 20～85, and the tower top pressure preferable range is 0.6～4.0MPaG; The reflux ratio preferable range is 1.2～3.5, and phegma temperature preferable range is-15～-60 ℃.The optimized technical scheme lightness-removing column adopts packing tower or tray column, and the theoretical tray sum preferable range of lightness-removing column is 10～60, and the tower top pressure preferable range is 0.7～4.2MPaG, and the feeding temperature preferable range is-15～-60 ℃.The heavy constituent that ethylene distillation Tata still is discharged get into earlier adiabatic flash jar middle part again after heat exchange.The service temperature preferable range of adiabatic flash jar is-15～80 ℃, and the pressure preferable range is 0.6～4.0MPaG.The heavy constituent that are circulated to the flash tank middle part in weight ratio are 50～200: 1 with the heavy constituent weight ratio preferable range of discharging out-of-bounds.
Among the present invention, the refining two tower separation process that adopted rectifying tower and lightness-removing column of ethene in the present technique, the major equipment of ethylene distillation system is an ethylene rectification tower, ethylene rectification tower is the packing tower or the valve tray column of an operation under pressurized conditions.This tower carries out rectifying to the crude ethylene from the ethene dehumidification system, realizes the separation of the ethene heavy constituent that its boiling point is high on year-on-year basis.In this tower, crucial light constituent is an ethene, and crucial heavy constituent are ethane, so overhead product is ethene and light constituent thereof, and still liquid is the heavy constituent that contain some amount ethene at the bottom of the tower.It mainly acts on is separating from cat head than light component such as the low-boiling hydrogen of ethene, methane, carbon monoxide and ethene in the charging crude ethylene, at the bottom of tower, discharging ethane, ether and C
3 +Above heavy constituent.Owing to after rectifying, adopted lightness-removing column; Can be from separating from cat head than light component such as the low-boiling hydrogen of ethene, methane, carbon monoxide in the charging crude ethylene of ethylene distillation column overhead; Can come the smart ethylene product that obtains at the bottom of the control tower according to the different demands in downstream; Can control the specification of quality of product flexibly, can significantly reduce the energy consumption of device simultaneously, obtain the better economic effect.Simultaneously and since adopted flash tank to ethylene distillation Tata still heavy constituent carry out adiabatic flash, the ethene amount that remains in the heavy constituent is reduced greatly, it is operated under pressurized conditions, the ethene that steams returns the ethylene rectification tower bottom; Its bottom then obtains the still liquid (heavy constituent) that ethylene content greatly reduces.Through evidence, adopt technical scheme of the present invention, the ethylene recovery rate of ethylene rectification tower reaches more than 98%, even near 100%, has obtained good technical effect.The adiabatic flash jar is for further reclaiming the specific equipment that the ethene in the ethylene distillation tower bottoms is provided with.
Description of drawings
Fig. 1 is the flow process of ethene separation method of the present invention.
Among Fig. 1,1 is the crude ethylene (mainly containing ethene, light constituent and heavy constituent) from reactive moieties, and 2 is ethylene compressor; 3 are the crude ethylene after the compression, and 4 is the crude ethylene water cooler, and 5 is cooled crude ethylene logistics; 6 is the ethene drying tower; 7 is dried crude ethylene logistics, and 8 is ethylene rectification tower, and 9 (mainly contain ethane, C for the ethylene distillation tower bottoms
3And above component), 10 is still liquid well heater, and 11 is the adiabatic flash jar; 12 are flash drum overhead logistics (ethene that contains a small amount of heavy constituent), 13 the still liquid that are circulated to the flash tank middle part for the discharge of flash tank bottom, and 14 for draining into flash tank bottoms (the still liquid that contains small amount of ethylene) out-of-bounds; 15 are ethylene rectification tower overhead stream (mainly containing ethene, light constituent); 16 is lightness-removing column, and 17 are lightness-removing column top logistics (mainly containing hydrogen, methane and carbon monoxide), and 18 is ethylene product.
Through embodiment the present invention is done further elaboration below.
Embodiment
[embodiment 1]
Crude ethylene from reactive system consists of: hydrogen 0.05kg/h, methane 2.17kg/h, carbon monoxide 3.70kg/h, ethanol 0.33kg/h, ethene 904.92kg/h, ethane 5.07kg/h, acetaldehyde 0.34kg/h, propylene 1.12kg/h, C
3 +4.43kg/h, ether 4.09kg/h, water 530.27kg/h.This crude ethylene logistics gets into the ethylene rectification tower middle and lower part after compression, cooling and drying, ethylene rectification tower is packing tower or tray column, has 84 blocks of theoretical trays; Wherein rectifying section is 48 blocks of column plates, and tower top pressure is 2.65MPaG, and tower top temperature is-17 ℃; Tower still pressure is 2.69MPaG; Tower still temperature is-2 ℃, and reflux ratio is 2.7, and the phegma temperature is-20 ℃.
As a result, obtain containing ethane, C at ethylene distillation Tata still
3And the ethylene distillation tower bottoms of above component, it consists of: ethanol 0.27kg/h, ethene 27.15kg/h, ethane 17.55kg/h, acetaldehyde 0.36kg/h, propylene 1.83kg/h, C
3 +5.08kg/h, ether 4.22kg/h, the therein ethylene weight concentration is 48.08%.This still liquid heater via heating back gets into the flash tank middle part and carries out adiabatic flash; The temperature of flash tank is 15 ℃; Pressure is 2.69MPaG; After the menopause heat-lightening steamed, flash drum overhead flashed off the material that mainly contains ethene and is recycled into the ethylene rectification tower bottom, and it consists of: ethene 21.93kg/h, ethane 12.50kg/h, acetaldehyde 0.02kg/h, propylene 0.71kg/h, C
3 +0.65kg/h, ether 0.13kg/h.The flash tank bottom discharge mainly contains ether, ethane, C
3, C
3 +With ethene etc.; The still liquid measure that is circulated to flash tank middle part is 100: 1 (weight ratio) with the ratio that drains into still liquid measure out-of-bounds, the consisting of of still liquid discharging: ethanol 0.27kg/h, ethene 5.22kg/h, ethane 5.05kg/h, acetaldehyde 0.34kg/h, propylene 1.12kg/h, C
3 +4.43kg/h, ether 4.09kg/h, then the ethylene recovery rate of ethylene rectification tower is 99.42%.
The discharging of ethylene distillation column overhead consists of: hydrogen 0.05kg/h, methane 11.71kg/h, carbon monoxide 9.00kg/h, carbonic acid gas 0.01kg/h, ethene 1782.52kg/h, ethane 0.23kg/h, water 0.02kg/h.This cat head material gets into the lightness-removing column top, steams light constituents such as containing hydrogen, methane and carbon monoxide from the lightness-removing column cat head again, obtains ethylene product from lightness-removing column tower still, and the purity of ethylene product is 99.9%.
[embodiment 2]
Press condition and the step of embodiment 1, ethylene rectification tower working pressure and temperature remain unchanged; The service temperature that changes flash tank is 20 ℃; Changing the still liquid measure that is circulated to the flash tank middle part is 120: 1 (weight ratio), then consisting of of still liquid discharging with the ratio that drains into still liquid measure out-of-bounds: ethanol 0.22kg/h, ethene 3.27kg/h, ethane 4.01kg/h, acetaldehyde 0.27kg/h, propylene 0.89kg/h, C
3 +3.51kg/h, ether 3.24kg/h, then the ethylene recovery rate of ethylene rectification tower is 99.63%, the purity of ethylene product is 99.92%.
[embodiment 3]
Press condition and the step of embodiment 1, the tower top pressure that changes ethylene rectification tower is 2.25MPaG, and then tower top temperature is-26 ℃, and tower still pressure is 2.29MPaG, and tower still temperature is-6 ℃, and reflux ratio is constant, and the phegma temperature is-30 ℃; The service temperature of flash tank is constant; Working pressure changes 2.25MPaG into; The still liquid measure that is circulated to the flash tank middle part is constant with the ratio that drains into still liquid measure out-of-bounds, then consisting of of still liquid discharging: ethanol 0.22kg/h, ethene 1.64kg/h, ethane 5.07kg/h, acetaldehyde 0.34kg/h, propylene 1.12kg/h, C
3 +4.43kg/h, ether 4.09kg/h, then the ethylene recovery rate of ethylene rectification tower is 99.82%, the purity of ethylene product is 99.95%.
[embodiment 4]
Press condition and the step of embodiment 1, the tower top pressure that changes ethylene rectification tower is 2.25MPaG, and then tower top temperature is-26 ℃, and tower still pressure is 2.29MPaG, and tower still temperature is-6 ℃, and reflux ratio is constant, and the phegma temperature is-30 ℃; The service temperature that changes flash tank is 20 ℃; Working pressure changes 2.25MPaG into; The still liquid measure that is circulated to the flash tank middle part is 120: 1 (weight ratio), then consisting of of still liquid discharging with the ratio that drains into still liquid measure out-of-bounds: ethanol 0.18kg/h, ethene 0.97kg/h, ethane 3.32kg/h, acetaldehyde 0.23kg/h, propylene 0.73kg/h, C
3 +2.90kg/h, ether 2.68kg/h, then the ethylene recovery rate of ethylene rectification tower is 99.89%, the purity of ethylene product is 99.96%.
[comparative example]
Press condition and the step of embodiment 1, remove the flash tank box dehydrogenation tower of ethylene distillation Tata still, then the ethylene recovery rate of ethylene rectification tower is 99%, and the purity of ethylene product is 99.3%.
Claims (8)
1. ethene separation method may further comprise the steps:
A) contain ethene, ethane and C
3And the mixture of above heavy constituent entering ethylene rectification tower middle and lower part, isolate the ethylene streams I that contains light constituent at cat head, the tower still is isolated and is mainly contained ethane, C
3And the heavy constituent logistics II of above component;
B) the logistics II drains into the flash tank middle part; Behind the flash tank adiabatic flash; Flash drum overhead discharge contain a small amount of heavy constituent ethene to the ethylene rectification tower bottom, the heavy constituent part circulation that discharge the flash tank bottom gets into the flash tank middle part, another part is discharged out-of-bounds;
C) the logistics I gets into the lightness-removing column top, obtains containing the light constituent of hydrogen, methane and carbon monoxide at cat head, and the tower still obtains ethylene product.
2. ethene separation method according to claim 1 is characterized in that ethylene rectification tower adopts packing tower or tray column.
3. ethene separation method according to claim 1 is characterized in that lightness-removing column adopts packing tower or tray column.
4. ethene separation method according to claim 1; The theoretical tray that it is characterized in that ethylene rectification tower adds up to 50～120, and wherein the rectifying section theoretical plate number is 20～85, and tower top pressure is 0.6～4.0MPaG; Reflux ratio is 1.2～3.5, and the phegma temperature is-15～-60 ℃.
5. ethene separation method according to claim 1 is characterized in that the theoretical tray of lightness-removing column adds up to 10～60, and tower top pressure is 0.7～4.2MPaG, and feeding temperature is-15～-60 ℃.
6. ethene separation method according to claim 1 is characterized in that the heavy constituent that ethylene distillation Tata still is discharged get into earlier adiabatic flash jar middle part again after heat exchange.
7. according to the said ethene separation method of claim 1, it is characterized in that the service temperature of adiabatic flash jar is-15～80 ℃, pressure is 0.6～4.0MPaG.
8. ethene separation method according to claim 1, the heavy constituent that it is characterized in that being circulated to the flash tank middle part are 50～200: 1 with the heavy constituent weight ratio of discharging out-of-bounds.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539605A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Separation method for preparing ethylene through ethanol dehydration |
| CN103664448A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Separating and refining method for preparing ethylene by dehydrating biomass ethanol |
| CN103772102A (en) * | 2012-10-17 | 2014-05-07 | 中国石油化工股份有限公司 | Separation refining method for ethylene preparation through ethanol dehydration |
| CN103772101A (en) * | 2012-10-17 | 2014-05-07 | 中国石油化工股份有限公司 | Separation refining method for ethylene preparation from ethanol |
| CN103827062A (en) * | 2011-07-28 | 2014-05-28 | 道达尔研究技术弗吕公司 | Process for removing oxygenated contaminants from an ethylene stream |
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| CN101648844A (en) * | 2009-08-30 | 2010-02-17 | 丰原宿州生物化工有限公司 | Preparation method of ethylene for refrigeration in condenser of light component removal column used in production of ethylene |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103827062A (en) * | 2011-07-28 | 2014-05-28 | 道达尔研究技术弗吕公司 | Process for removing oxygenated contaminants from an ethylene stream |
| CN103827062B (en) * | 2011-07-28 | 2016-05-11 | 道达尔研究技术弗吕公司 | For removing the method containing oxygen contamination thing from ethylene streams |
| CN103539605A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Separation method for preparing ethylene through ethanol dehydration |
| CN103539605B (en) * | 2012-07-12 | 2015-12-16 | 中国石油化工股份有限公司 | The separation method of producing ethylene from dehydration of ethanol |
| CN103664448A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Separating and refining method for preparing ethylene by dehydrating biomass ethanol |
| CN103772102A (en) * | 2012-10-17 | 2014-05-07 | 中国石油化工股份有限公司 | Separation refining method for ethylene preparation through ethanol dehydration |
| CN103772101A (en) * | 2012-10-17 | 2014-05-07 | 中国石油化工股份有限公司 | Separation refining method for ethylene preparation from ethanol |
| CN103772102B (en) * | 2012-10-17 | 2015-08-12 | 中国石油化工股份有限公司 | The separation and refining method of producing ethylene from dehydration of ethanol |
| CN103772101B (en) * | 2012-10-17 | 2016-04-13 | 中国石油化工股份有限公司 | The separation and refining method of producing ethylene with ethyl alcohol |
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