CN103420751A - Method for removing light component in ethylene preparation process through ethanol dehydration - Google Patents
Method for removing light component in ethylene preparation process through ethanol dehydration Download PDFInfo
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- CN103420751A CN103420751A CN2012101502063A CN201210150206A CN103420751A CN 103420751 A CN103420751 A CN 103420751A CN 2012101502063 A CN2012101502063 A CN 2012101502063A CN 201210150206 A CN201210150206 A CN 201210150206A CN 103420751 A CN103420751 A CN 103420751A
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Abstract
The present invention relates to a method for removing a light component in an ethylene preparation process through ethanol dehydration, wherein problems of low ethylene yield and high energy consumption as described in the previous literature are mainly solved according to the present invention. The technical scheme comprises that the liquid phase on the top of an ethylene rectification tower is extracted, the extracted liquid phase enters a light component rectification tower, an ethylene-containing light component is separated from the tower top, the ethylene-containing light component is condensed, the gas phase is externally discharged, the liquid phase completely refluxes to the light component rectification tower, and the ethylene product is obtained from the tower kettle. With the technical scheme, the problems are well solved, and the method can be used for industrial production of ethylene preparation through ethanol dehydration.
Description
Technical field
The present invention relates to remove in a kind of producing ethylene from dehydration of ethanol technique the method for light constituent.
Background technology
Ethene is a kind of important large organic chemical industry's basic raw material, is mainly used to produce the multiple Organic chemical products such as polyethylene, polyvinyl chloride, ethylene oxide/ethylene glycol, ethyl benzene/styrene, vinyl acetate between to for plastic.At present, ethylene production mainly adopts the production of petroleum catalystic pyrolysis both at home and abroad.In recent years the research of non-petroleum production ethene had to new breakthrough, particularly the producing ethylene by ethanol dehydration technology.This technology be the ethanol that derives from agricultural byproducts be raw material, can avoid the dependence to petroleum resources like this.To oil-poor and take agricultural and be main country and regional, the raw material of producing ethanol is easy to get and is guaranteed, for producing ethene, has established enough raw material bases, can solve fossil resource shortage and the serious difficult problem of environmental pollution.
Producing ethylene with ethyl alcohol, its key factor is to study the strong technique with having the market competitiveness of a kind of new economy, and main goal in research is to improve technical process, reduces the ethanol unit consumption, increases the device benefit.
In the processing method of producing ethylene from dehydration of ethanol, at home and abroad oneself has many methods in disclosed document or patent, and its basic technology mainly is divided into fixed-bed process and fluidized-bed process.ABB Lummu: company once proposed to carry out ethanol dehydration reaction preparing ethylene (USP4134926) by fluidization at late nineteen seventies, but this technology not yet obtains industrial applications.At present industrial application be mainly fixed-bed process, comprise isothermal fixed-bed process and insulation fix bed technique.
Initial ethanol dehydration reaction carries out in calandria type fixed bed, and reaction pressure is normal pressure, adopts direct heating or utilizes the mode of heating medium (as fused salt) indirect heating to provide reaction heat for reaction.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 other by products, if but increase flow velocity, the transformation efficiency of ethanol can drop to again and solve this contradiction, United States Patent (USP) (USP4232179) has proposed skill in the thermal insulation of ethanol dehydration reaction, be that ethanol dehydration reaction carries out in insulation fix bed, it is temperature required that reaction mass is heated to reaction before entering reactor, to guarantee normally carrying out of reaction.Afterwards, they have proposed again the insulation fix bed reaction process of syllogic (USP4396789), and utilize this technique to set up 60,000 ton/years of ethylene units in the early 1980s.The insulation fix bed reactor of three series connection of this process using, come ethanol and the vapor mixing charging of each Reactor inlet of preheating with a stove, the by products such as unreacted ethanol and ether are carried out circulation.Adding of steam reduced the reaction coking, extended the life-span of catalyzer, improved productive rate.Install service data and show, when reactor inlet temperatures is 450 ℃, ethanol conversion reaches 98, at least one year of catalyst regeneration cycle.In addition Halcon/SD company and tenth century the seventies developed the double mode technology of thermal insulation or isothermal fixed bed, wherein the isothermal bed technology has obtained industrial applications.The device service data shows: in 318 ℃ of temperature of reaction, liquid air speed (LHSV) 0.23 hour
-1Condition under, ethylene selectivity 96.8% (mole), ethanol conversion 99.1%, 8 months catalyst regeneration cycles.After, Halcon/SD company has developed again multistage insulation fixed bed reaction process: ethanol dewaters and generates ethene enters multistage insulation fixed bed reaction after the water vapor dilution in, reactant gases carries out low temperature fractionation after washing, compression, alkali cleaning and drying again, finally obtains the polymer grade ethylene product.The examination data show: 465 ℃ of temperature of reaction, and liquid air speed (LHSV) 0.8 hour
-1And steam: under the condition that the ethanol ratio is 3:1, ethylene selectivity 99.4% (mole), ethanol conversion 99.9%, 8 months catalyst regeneration cycles.Lummus company has realized the industrialization of fixed-bed process as far back as nineteen sixties.This process using shell and tube isothermal reactor, adopt thermal oil system to provide reaction required heat.The one Al catalysts regeneration period of silicon is 3 weeks, and every regeneration once needs 3 days.Under 315 ℃ of temperature of reaction, reaction pressure 0.16MPa condition, ethylene selectivity approximately 94% (mole), ethanol conversion 99%.
In existing document or report, in shorter mention ethene Dehydration ethene, the removing process of light constituent reaches the problem that how to improve yield of ethene, reduces energy consumption.The separating technology of full scale plant is to adopt two tower flow processs at present, and crude ethylene is introduced into ethylene rectification tower, and tower top light constituent gas phase after partial condensation effluxes, and liquid phase is delivered to light constituent stripping tower top, removes the light constituent in liquid phase, to obtain 99.99% smart ethene., though can obtain 99.99% smart ethene, owing to adopting tower top charging, stripping distil process to remove light constituent, there is the problem that ethylene loss and energy consumption are high in this technique.The invention provides a kind of lights removal technique of new producing ethylene from dehydration of ethanol, the method has that ethylene recovery efficiency is high, energy consumption is low, the characteristics of good product quality.
Summary of the invention
Technical problem to be solved by this invention is to have the problem that yield of ethene is low, energy consumption is high in previous literature, and a kind of method that removes light constituent in new producing ethylene from dehydration of ethanol technique is provided.The method has advantages of that ethylene recovery efficiency is high, energy consumption is low, good product quality.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method that removes light constituent in producing ethylene from dehydration of ethanol technique, the ethene that contains methane, carbon monoxide, hydrogen light constituent enters light constituent rectifying tower middle part, at tower top, isolate containing the ethene light constituent, liquid phase total reflux after condensation, the vapour phase light constituent effluxes, and in the bottom of light constituent rectifying tower, obtains the liquid phase ethylene product.
In technique scheme, the service temperature preferable range of light constituent rectifying tower is-45.0～-10.0 ℃, and the working pressure preferable range is 1.2～4.3MpaG.The theoretical plate number preferable range of light constituent rectifying tower is 2～60, and the feed entrance point preferred version is at 2～58 theoretical tray places.
In the lights removal technique of producing ethylene from dehydration of ethanol of the present invention, the light constituent liquid phase that contains ethene from the ethylene distillation column overhead is delivered to the middle part of light constituent rectifying tower, the overhead stream of light constituent rectifying tower is after partial condensation, liquid-phase reflux is to the light constituent rectifying tower, gas phase effluxes, and obtains 99.99% smart ethene in the bottom of light constituent rectifying tower.
Owing to adopting the light constituent rectifying tower to be made with extra care the light constituent in ethene, remove the light constituent in ethene in the present invention, thereby avoided ethylene component more in former technique to circulate between lightness-removing column and ethylene rectification tower on the one hand, reduced energy consumption; Can make again on the other hand fully separating of ethene and light constituent, yield of ethene increases, and product purity is further made with extra care.Adopt technical scheme of the present invention through evidence, the crude ethylene separating energy consumption reduces by 14.32%, and unit ton ethylene product increases ethylene yield 3kg, and ethylene product purity is further enhanced, and has obtained technique effect preferably.
The accompanying drawing explanation
Fig. 1 removes the method flow schematic diagram of light constituent in producing ethylene from dehydration of ethanol technique of the present invention.
Fig. 2 is the schematic flow sheet of the separating technology of existing producing ethylene from dehydration of ethanol full scale plant.
In Fig. 1,1 is the ethene that contains light constituent from the ethylene distillation column overhead, 2 for containing finite concentration ethene light constituent rectifying tower tower top vapor-phase material, 3 is the backflow of light constituent rectifying tower, 4 for the light constituent rectifying tower effluxes the vapour phase light constituent, and 5 is ethylene product, the condenser that 1a is the light constituent rectifying tower, the return tank that 2a is the light constituent rectifying tower, 3a is the light constituent rectifying tower.
In Fig. 2, 1 is the crude ethylene from the ethene dehumidification system, 2 is the tower reactor heavy constituent that contains finite concentration ethene ethylene rectification tower, the 3 tower top materials that are ethylene rectification tower, 4 backflows that are ethylene rectification tower, 5 is ethylene product, 6 phlegmas that are ethylene rectification tower and light constituent stripping tower, 7 backflows that are cut light tower, the 8 tower top materials that are cut light tower, 9 is outer exhaust phase light constituent, 10 is the discharging of ethylene rectification tower return tank vapour phase, the liquid phase of 11 condensers that are lights column, 1a is ethylene rectification tower, 2a is the ethylene rectification tower reflux pump, 3a is the light constituent stripping tower, the condenser that 4a is ethylene rectification tower, the return tank that 5a is ethylene rectification tower, the condenser that 6a is the light constituent stripping tower, the reboiler that 7a is the light constituent stripping tower.
Below by embodiment, the present invention is further elaborated.
Embodiment
[embodiment 1]
Press the schematic flow sheet of Fig. 1, enter ethylene rectification tower from the crude ethylene of ethene dehumidification system and separated, separate the ethene that contains light constituent at tower top, in tower reactor, isolate heavy constituent.Each composition flow rate of crude ethylene is: 0.070 kg/hr of hydrogen, 0.070 kg/hr, methane, 0.557 kg/hr of carbon monoxide, 1274.518 kg/hrs of ethene, 7.060 kg/hrs, ethane, 1.555 kg/hrs, propane, 0.113 kg/hr, acetaldehyde, 5.631 kg/hrs of ether, 33.957 kg/hrs of heavy constituents.The charging of light constituent rectifying tower is 1261.450 kg/hrs, wherein containing 1260.743 kg/hrs of ethene.The tower top temperature of light constituent rectifying tower is-23 ℃, and pressure is 2.35MPaG, and the tower reactor temperature is-21.6 ℃, and full tower theoretical plate number is 18, and feed entrance point is in middle and upper part.After distillation, tower top steams light constituent material containing ethene through partial condensation, vapor-liquid separation, and liquid phase is returned to the light constituent rectifying tower as backflow, and gas phase effluxes, and flow is 7.820 kg/hrs, containing ethene, is wherein 7.137 kg/hrs.The bottom extraction essence ethylene product of light constituent rectifying tower, flow is 1253.603 kg/hrs, ethene purity reaches 99.998%.The condenser heat load of ethylene rectification tower is 430.376kw, and the condenser heat load of light constituent rectifying tower is 28.867kw.
[embodiment 2]
With embodiment 1, only change theoretical stage and the charging version position of light constituent rectifying tower: full tower theoretical plate number is 12, and feed entrance point is in middle and upper part, the other the same as in Example 1.The charging of light constituent rectifying tower is 1261.450 kg/hrs.It is 7.790 kg/hrs that the light constituent rectifying tower top gaseous phase effluxes flow, containing ethene, is wherein 7.112 kg/hrs, the bottom extraction essence ethylene product of light constituent rectifying tower, and flow is 1253.672 kg/hrs, ethene purity reaches 99.998%.The tower top temperature of light constituent rectifying tower is-22.7 ℃, and pressure is 2.35MPaG, and the tower reactor temperature is-21.6 ℃, and the condenser heat load of light constituent rectifying tower is 28.867kw.
[embodiment 3]
With embodiment 1, only change the working pressure of light constituent rectifying tower: tower top pressure 2.55 MPaG, the other the same as in Example 1.The charging of light constituent rectifying tower is 1261.450 kg/hrs.It is 6.056 kg/hrs that the light constituent rectifying tower top gaseous phase effluxes flow, containing ethene, is wherein 5.382 kg/hrs, the bottom extraction essence ethylene product of light constituent rectifying tower, and flow is 1255.381 kg/hrs, ethene purity reaches 99.997%.The tower top temperature of light constituent rectifying tower is-20.1 ℃, and pressure is 2.55MPaG, and the tower reactor temperature is-18.5 ℃, and the condenser heat load of light constituent rectifying tower is 23.089kw.
[comparative example]
Press the schematic flow sheet of Fig. 2, enter ethylene rectification tower from the crude ethylene of ethene dehumidification system and separated, separate the ethene that contains light constituent at tower top, in tower reactor, isolate heavy constituent.Each composition flow rate of crude ethylene is the same, and the restructuring of ethylene rectification tower tower reactor is divided into 62.082 kg/hrs, and therein ethylene is 13.765 kg/hrs.Ethylene distillation column overhead light constituent is 5510.374 kg/hrs, therein ethylene is 5502.95 kg/hrs, after condensation, is divided into two strands, the backflow of ethylene rectification tower is 4248.924 kg/hrs, and the charging of light constituent stripping tower is 1573.673 kg/hrs.The tower top temperature of light constituent stripping tower is-22.4 ℃, and pressure is 2.35MPaG, and the tower reactor temperature is-21.6 ℃, and full tower theoretical plate number is 18, and feed entrance point is at top.After stripping, tower top steams the uncooled light constituent mixing of materials containing the light constituent material of ethene and ethylene rectification tower, through partial condensation, vapor-liquid separation, liquid phase is mixed with the overhead condensation liquid of ethylene rectification tower, gas phase effluxes, flow is 11.422 kg/hrs, containing ethene, is wherein 10.763 kg/hrs.The bottom extraction essence ethylene product of light constituent stripping tower, flow is 1250.053 kg/hrs, ethene purity reaches 99.996%.The condenser heat load of ethylene rectification tower is 507.888kw, and the thermal load of light constituent condenser is 28.712kw.
Claims (3)
1. remove the method for light constituent in a producing ethylene from dehydration of ethanol technique, the ethene that contains methane, carbon monoxide, hydrogen light constituent enters light constituent rectifying tower middle part, at tower top, isolate containing the ethene light constituent, liquid phase total reflux after condensation, the vapour phase light constituent effluxes, and in the bottom of light constituent rectifying tower, obtains the liquid phase ethylene product.
2. remove according to claim 1 the method for light constituent in a kind of producing ethylene from dehydration of ethanol technique, the service temperature that it is characterized in that the light constituent rectifying tower is-45.0～-10.0 ℃, and working pressure is 1.2～4.3MpaG.
3. remove according to claim 1 the method for light constituent in a kind of producing ethylene from dehydration of ethanol technique, the theoretical plate number that it is characterized in that the light constituent rectifying tower is 2～60, and feed entrance point is at 2～58 theoretical tray places.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306973A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Process for recovering ethylene in process of ethylene preparation by ethanol dehydration |
| CN102372558A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for preparing ethylene by using ethanol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306973A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Process for recovering ethylene in process of ethylene preparation by ethanol dehydration |
| CN102372558A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for preparing ethylene by using ethanol |
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Application publication date: 20131204 |