CN103772102B - The separation and refining method of producing ethylene from dehydration of ethanol - Google Patents
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Abstract
The present invention relates to a kind of separation and refining method of producing ethylene from dehydration of ethanol, mainly solve the problem that separation, particularly yield of ethene are low, energy consumption is low not relating to product in producing ethylene from dehydration of ethanol in previous literature.The present invention enters ethylene rectification tower by adopting containing the mixture of ethene, ethane and carbon three and above hydrocarbon thereof and light constituent, and isolate the ethene containing light constituent at tower top, vapour phase enters cut light tower, is rich in the heavy constituent of ethene in tower reactor discharge; Containing the vapour phase ethene of light constituent after cut light tower is refining, overhead vapor phase separates vapour phase light constituent through condensation, phlegma returns cut light tower as backflow, and deliver to the top of ethylene rectification tower through pump pressure part as backflow in the bottom liquid phases of cut light tower, all the other are ethylene product; The heavy constituent being rich in ethene enters the top of heavy constituent stripping distillation tower, stripping overhead vapour phase returns to the middle and lower part of ethylene rectification tower, obtain the technical scheme of the heavy constituent containing a small amount of ethene at the bottom of tower, solve this problem preferably, can be used in producing ethylene from dehydration of ethanol industrial production.
Description
Technical field
The present invention relates to a kind of separation and refining method of producing ethylene from dehydration of ethanol.
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, domestic and international ethylene production mainly adopts petroleum catalystic pyrolysis to produce.New breakthrough was had, particularly producing ethylene by ethanol dehydration technology in recent years to the research of non-petroleum feedstocks production ethene.This technology derives from the ethanol of agricultural byproducts for raw material, can avoid the dependence to petroleum resources like this.To oil-poor and country based on agricultural and area, the raw material producing ethanol is easy to get and guaranteed, has established enough raw material bases for producing ethene, 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 improving technique flow process, reduces ethanol unit consumption, increases 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 is mainly divided into fixed-bed process and fluidized-bed process.ABB Lummu: company once carried out ethanol dehydration reaction preparing ethylene (USP4134926) in late nineteen seventies proposition fluidization, but this technology not yet obtains industrial applications.Current 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 reacting.In reaction process, temperature of reaction and material flow are key factors, if temperature is too high or material flow is too low, the generation of other by products will be caused, if but increase flow velocity, the transformation efficiency of ethanol can drop to again and solve this contradiction, skill in the thermal insulation that United States Patent (USP) (USP4232179) proposes ethanol dehydration reaction, namely ethanol dehydration reaction carries out in insulation fix bed, it is temperature required that reaction mass is heated to reaction before entering the reactor, to ensure normally carrying out of reaction.Afterwards, they also been proposed the insulation fix bed reaction process of syllogic (USP4396789), and utilize this technique to set up 60,000 tons/year of ethylene units in the early 1980s.This technique adopts three insulation fix bed reactors of connecting, and comes ethanol and the vapor mixing charging of each Reactor inlet of preheating with a stove, and the by products such as unreacted ethanol and ether carry out circulation.Adding of steam decreases reaction coking, extends the life-span of catalyzer, improves productive rate.Plant running data show, when reactor inlet temperatures is 450 DEG C, ethanol conversion reaches 98, catalyst regeneration cycle at least one year.In addition Halcon/SD company and tenth century the seventies develop the double mode technology of thermal insulation or isothermal fixed bed, wherein isothermal bed technology obtains industrial applications.Plant running data show: in temperature of reaction 318 DEG C, liquid air speed (LHSV) 0.23 hour
-1condition under, ethylene selectivity 96.8% (mole), ethanol conversion 99.1%, catalyst regeneration cycle 8 months.After, Halcon/SD company develops again multistage insulation fixed bed reaction process: ethanol enters dehydration in multistage insulation fixed bed reaction and generates ethene after steam dilution, reactant gases carries out low temperature fractionation again after washing, compression, alkali cleaning and drying, finally obtains polymer grade ethylene product.Examination data show: temperature of reaction 465 DEG C, liquid air speed (LHSV) 0.8 hour
-1and steam: under the condition that ethanol ratio is 3:1, ethylene selectivity 99.4% (mole), ethanol conversion 99.9%, catalyst regeneration cycle 8 months.Lummus company achieves the industrialization of fixed-bed process as far back as nineteen sixties.This technique adopts shell and tube isothermal reactor, and employing thermal oil system provides the heat needed for reaction.The silicon one Al catalysts regeneration period is 3 weeks, often regenerates and once needs 3 days.Under temperature of reaction 315 DEG C, reaction pressure 0.16MPa condition, ethylene selectivity about 94% (mole), ethanol conversion 99%.
In existing document or report, how the problem of the separating technology of product in shorter mention ethene Dehydration ethene, particularly improve yield of ethene, reduce the technical problem such as energy consumption.The separating technology of current full scale plant adopts two-tower process, and crude ethylene is introduced into ethylene rectification tower, and tower top light constituent gas phase after partial condensation is arranged outward, and liquid phase delivers to light constituent stripping tower, removes the light constituent in liquid phase, to obtain 99.99% smart ethene.This technique, adopts double-column process, there is the problem that technique is comparatively complicated, energy consumption is higher.Patent (ZL200710040705.64) proposes the method adopting adiabatic flash, and the ethene in recovered ethylene rectifying tower bottoms, though recyclable part ethene, organic efficiency is not high.The invention provides a kind of separating technology of new producing ethylene from dehydration of ethanol, the method has the advantages that ethylene recovery efficiency is high, energy consumption is low.
Summary of the invention
Technical problem to be solved by this invention is the separating technology problem not relating to product in producing ethylene from dehydration of ethanol in previous literature, particularly how to improve yield of ethene, reduce the technical problem of energy consumption, a kind of separation and refining method of new producing ethylene from dehydration of ethanol is provided.The yield that the method has ethene is high, and energy consumption is low, the advantage that ethylene product purity is high.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of separation and refining method of producing ethylene from dehydration of ethanol, ethylene rectification tower is entered containing the mixture of ethene, ethane and carbon three and above hydrocarbon thereof and light constituent, the ethene containing light constituent is isolated at tower top, vapour phase enters cut light tower, discharges the heavy constituent being rich in ethene in tower reactor; Containing the vapour phase ethene of light constituent after cut light tower is refining, overhead vapor phase separates vapour phase light constituent through condensation, phlegma returns cut light tower as backflow, and deliver to the top of ethylene rectification tower through pump pressure part as backflow in the bottom liquid phases of cut light tower, all the other are ethylene product; The heavy constituent being rich in ethene enters the top of heavy constituent stripping distillation tower, and stripping overhead vapour phase returns to the middle and lower part of ethylene rectification tower, obtains the heavy constituent containing a small amount of ethene at the bottom of tower.
In technique scheme, the service temperature preferable range of ethylene rectification tower is-35 ~ 30.0 DEG C, working pressure preferable range is 1.3 ~ 4.5MPaG, and theoretical plate number preferable range is 50 ~ 140, and crude ethylene feed entrance point preferable range is at 40 ~ 110 theoretical tray places.The service temperature preferable range of cut light tower is-45.0 ~-10.0 DEG C, and working pressure preferable range is 1.2 ~ 4.3MPaG, and theoretical plate number preferable range is 2 ~ 60.The service temperature preferable range of heavy constituent stripping distillation tower is-15 ~ 80 0 DEG C, and working pressure preferable range is 1.0 ~ 4.0MPaG, and theoretical plate number preferable range is 2 ~ 50, and feed entrance point is at top.Stripping overhead vapour phase returns the feed entrance point preferable range of ethylene rectification tower at 39 ~ 140 theoretical tray places.The liquid phase of cut light tower tower reactor extraction is divided into two strands of materials: the backflow of ethylene rectification tower and ethylene product, and the part by weight preferable range of two strands of materials is 1 ~ 6:1, and preferable range is 2 ~ 4:1.
In technique scheme, the heavy constituent being rich in ethene enters the top of heavy constituent stripping distillation tower, and stripping overhead vapour phase returns to the middle and lower part of ethylene rectification tower, and the heavy constituent containing a small amount of ethene at the bottom of tower can be selected outer row or separately use it for anything else.Containing the vapour phase ethene of light constituent after cut light tower is refining, overhead vapor phase separates vapour phase light constituent through condensation and can select outer row or separately use it for anything else.Light constituent described in the present invention mainly refers to hydrogen, methane, carbon monoxide.
Owing to adopting double tower coupling path combination heavy constituent stripping distillation tower to refine crude ethylene in the present invention, remove the light constituent in ethene and heavy constituent, improve yield of ethene, reduce energy consumption, product purity is further enhanced; The ethylene content in ethylene distillation tower reactor liquid can be allowed greatly to increase on the other hand, ethylene rectification tower be operated and is more prone to.Prove to adopt technical scheme of the present invention through test, crude ethylene separating energy consumption reduces by 19.26%, the ethene amount remained in heavy constituent is reduced to 3% from 22%, and ethylene product purity can reach more than 99.99% and be further enhanced with yield, achieves good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the separation and refining method of producing ethylene from dehydration of ethanol of the present invention.
Fig. 2 is the schematic flow sheet of the separating technology of producing ethylene from dehydration of ethanol full scale plant.
In Fig. 1, 1 is the crude ethylene from ethene dehumidification system, 2 is the tower reactor heavy constituent containing finite concentration Ethylene vinyl rectifying tower, 3 is the tower top material of ethylene rectification tower, 4 is the backflow of ethylene rectification tower, 5 is ethylene product, 6 is the tower reactor liquid phase discharging of cut light tower, 7 is the backflow of cut light tower, 8 is the tower top material of cut light tower, 9 is outer exhaust phase light constituent, 10 is heavy constituent stripping overhead vapor-phase material, 11 is the tower reactor heavy constituent of heavy constituent stripping distillation tower, 1a is ethylene rectification tower, 2a is cut light tower tower reactor extraction pump, 3a is cut light tower, 4a is the condenser of cut light tower, 5a is the return tank of cut light tower, 6a is heavy constituent stripping distillation tower.
In Fig. 2, 1 is the crude ethylene from ethene dehumidification system, 2 is the tower reactor heavy constituent containing finite concentration Ethylene vinyl rectifying tower, 3 is the tower top material of ethylene rectification tower, 4 is the backflow of ethylene rectification tower, 5 is ethylene product, 6 is the phlegma of ethylene rectification tower and light constituent stripping tower, 7 is the backflow of cut light tower, 8 is the tower top material of cut light tower, 9 is outer exhaust phase light constituent, 10 is the discharging of ethylene rectification tower return tank vapour phase, 11 is the liquid phase of the condenser of lights column, 1a is ethylene rectification tower, 2a is ethylene rectification tower reflux pump, 3a is light constituent stripping tower, 4a is the condenser of ethylene rectification tower, 5a is the return tank of ethylene rectification tower, 6a is the condenser of light constituent stripping tower, 7a is the reboiler of light constituent stripping tower.
Below by embodiment, the present invention is further elaborated.
Embodiment
[embodiment 1]
Crude ethylene from ethene dehumidification system enters ethylene rectification tower and is separated, and separates the ethene containing light constituent, isolate heavy constituent in tower reactor at tower top.The each composition flow rate of crude ethylene is: hydrogen 0.070 kg/hr, 0.070 kg/hr, methane, carbon monoxide 0.557 kg/hr, ethene 1274.518 kgs/hr, 7.060 kgs/hr, ethane, 1.555 kgs/hr, propane, 0.113 kg/hr, acetaldehyde, ether 5.631 kgs/hr, heavy constituent 33.957 kgs/hr.The restructuring of ethylene rectification tower tower reactor is divided into 83.977 kgs/hr, and wherein ethene is 18.618 kgs/hr.Ethylene rectification tower overhead vapor phase enters the bottom of cut light tower, and flow is 5060.536 kgs/hr.The tower top temperature of ethylene rectification tower is-24.8 DEG C, and pressure is 2.15MPaG, and bottom temperature is 9.5 DEG C, and full tower theoretical plate number is 80, and feed entrance point is in middle and lower part.
Stripping distillation is carried out at the top that ethylene rectification tower tower reactor heavy constituent delivers to stripping distillation tower through pump pressure, and the tower top temperature of stripping distillation tower is 9.8 DEG C, and pressure is 2.17MPaG, and bottom temperature is 59.3 DEG C, and full tower theoretical plate number is 12.After stripping distillation, tower top steams the main Matter Transfer containing ethene and enters ethylene rectification tower bottom, and flow is 33.977 kgs/hr, and tower bottom is discharged main containing ethane and C
3 +mixture, flow is 50.0 kgs/hr, wherein containing ethene 1.692 kgs/hr.The thermal load of stripping distillation tower reboiler is 4.702kw.
The tower top temperature of cut light tower is-25.5 DEG C, and pressure is 2.14MPaG, and bottom temperature is-24.9 DEG C, and full tower theoretical plate number is 18, the vapour phase feed entrance point of ethylene distillation tower top in bottom, without reboiler.After distillation, tower top steams light constituent material containing ethene through partial condensation, vapor-liquid separation, and liquid phase returns cut light tower as backflow, and gas phase is arranged outward, and flow is 11.280 kgs/hr, is wherein 10.607 kgs/hr containing ethene.The bottom extraction of cut light tower, through pump pressure, is divided into two-way, and a road is as smart ethylene product.Another road is as the backflow of ethylene rectification tower, and to the top of ethylene rectification tower, flow is 3787.004 kgs/hr, and ethylene product flow is 1262.335 Grams Per Hours, and purity reaches 99.997%.The condenser heat load of cut light tower is 437.038kw.
Separation and purification technique yield of ethene is 99.04% (weight).
[embodiment 2]
With embodiment 1, the theoretical stage of a change ethylene rectification tower: full tower theoretical plate number is 92, feed entrance point in middle and lower part, the other the same as in Example 1.The restructuring of ethylene rectification tower tower reactor is divided into 84.035 kgs/hr, and wherein ethene is 18.631 kgs/hr.Ethylene rectification tower overhead vapor phase flow is 5061.121 kgs/hr, and the tower top temperature of ethylene rectification tower is-24.8 DEG C, and pressure is 2.15MPaG, and bottom temperature is 9.5 DEG C.
Stripping overhead steams the main Matter Transfer containing ethene and enters ethylene rectification tower bottom, and flow is 34.036 kgs/hr, and tower bottom is discharged main containing ethane and C
3 +mixture, flow is 50.0 kgs/hr, wherein containing ethene 1.686 kgs/hr.Carrying distillation tower column overhead temperatures is 9.8 DEG C, and pressure is 2.17MPaG, and bottom temperature is 59.3 DEG C.The thermal load of stripping distillation tower reboiler is 4.709kw.
Cut light tower vapour phase effluent stream amount is 11.275 kgs/hr, and wherein containing ethene is 10.604 kgs/hr.The bottom extraction of cut light tower is 3787.588 kgs/hr to the return flow of ethylene rectification tower, and ethylene product flow is 1262.529 Grams Per Hours, and purity reaches 99.998%.Tower top temperature is-25.5 DEG C, and pressure is 2.14MPaG, and bottom temperature is-24.9 DEG C.The condenser heat load of qi exhaustion lights column is 437.091kw.
Separation and purification technique yield of ethene is 99.06% (weight).
[embodiment 3]
With embodiment 1, the theoretical stage of a change stripping distillation tower: full tower theoretical plate number is 20, the other the same as in Example 1.The restructuring of ethylene rectification tower tower reactor is divided into 82.667 kgs/hr, and wherein ethene is 18.327 kgs/hr.Ethylene rectification tower overhead vapor phase flow is 5059.727 kgs/hr, and the tower top temperature of ethylene rectification tower is-24.8 DEG C, and pressure is 2.15MPaG, and bottom temperature is 10.0 DEG C.
Stripping overhead steams the main Matter Transfer containing ethene and enters ethylene rectification tower bottom, and flow is 32.667 kgs/hr, and tower bottom is discharged main containing ethane and C
3 +mixture, flow is 50.0 kgs/hr, wherein containing ethene 1.691 kgs/hr.Carrying distillation tower column overhead temperatures is 10.1 DEG C, and pressure is 2.17MPaG, and bottom temperature is 59.3 DEG C.The thermal load of stripping distillation tower reboiler is 4.568kw.
Cut light tower vapour phase effluent stream amount is 11.265 kgs/hr, and wherein containing ethene is 10.594 kgs/hr.The bottom extraction of cut light tower is 3786.194 kgs/hr to the return flow of ethylene rectification tower, and ethylene product flow is 1262.065 Grams Per Hours, and purity reaches 99.997%.Tower top temperature is-25.5 DEG C, and pressure is 2.14MPaG, and bottom temperature is-24.9 DEG C.The condenser heat load of qi exhaustion lights column is 436.973kw.
Separation and purification technique yield of ethene is 99.03% (weight).
[comparative example 1]
Crude ethylene from ethene dehumidification system enters ethylene rectification tower and is separated, and separates the ethene containing light constituent, isolate heavy constituent in tower reactor at tower top.The each composition flow rate of crude ethylene is the same, and the restructuring of ethylene rectification tower tower reactor is divided into 62.082 kgs/hr, and wherein ethene is 13.765 kgs/hr.Ethylene distillation column overhead light constituent is 5510.374 kgs/hr, wherein ethene is 5502.95 kgs/hr, after condensation, is divided into two strands, the backflow of ethylene rectification tower is 4248.924 kgs/hr, and the charging of light constituent stripping tower is 1573.673 kgs/hr.The tower top temperature of light constituent stripping tower is-22.4 DEG C, and pressure is 2.35MPaG, and bottom temperature is-21.6 DEG C, 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 of light constituent material containing ethene and ethylene rectification tower, through partial condensation, vapor-liquid separation, liquid phase mixes with the overhead condensation liquid of ethylene rectification tower, gas phase is arranged outward, flow is 11.422 kgs/hr, and wherein containing ethene is 10.763 kgs/hr.The bottom extraction essence ethylene product of light constituent stripping tower, flow is 1250.053 kgs/hr, and Ethylene 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.
[comparative example 2]
Crude ethylene from ethene dehumidification system enters ethylene rectification tower and is separated, and separates the ethene containing light constituent, isolate heavy constituent in tower reactor at tower top.The each composition flow rate of crude ethylene is the same.Ethylene rectification tower tower reactor heavy constituent delivers to adiabatic flash tank through pump pressure, heating.Flash drum overhead gas phase returns ethylene distillation tower bottom, extraction liquid phase heavy constituent bottom flash tank, each composition flow rate is: ethene 4.415 kgs/hr, 7.068 kgs/hr, ethane, 1.555 kgs/hr, propane, 0.113 kg/hr, acetaldehyde, ether 5.630 kgs/hr, heavy constituent 33.956 kgs/hr.The thermal load of well heater is 10.864kw, and yield of ethene is 98.80% (weight).
Claims (7)
1. the separation and refining method of a producing ethylene from dehydration of ethanol, ethylene rectification tower is entered containing the mixture of ethene, ethane and carbon three and above hydrocarbon thereof and light constituent, isolate the ethene containing light constituent at tower top, vapour phase enters cut light tower, discharges the heavy constituent being rich in ethene in tower reactor; Containing the vapour phase ethene of light constituent after cut light tower is refining, overhead vapor phase separates vapour phase light constituent through condensation, phlegma returns cut light tower as backflow, and deliver to the top of ethylene rectification tower through pump pressure part as backflow in the bottom liquid phases of cut light tower, all the other are ethylene product; The heavy constituent being rich in ethene enters the top of heavy constituent stripping distillation tower, and stripping overhead vapour phase returns to the middle and lower part of ethylene rectification tower, obtains the heavy constituent containing a small amount of ethene at the bottom of tower;
The service temperature of described heavy constituent stripping distillation tower is-15 ~ 800 DEG C, and working pressure is 1.0 ~ 4.0MPaG, and theoretical plate number is 2 ~ 50;
The liquid phase of described cut light tower tower reactor extraction is divided into two strands of materials: the backflow of ethylene rectification tower and ethylene product, and the part by weight of two strands of materials is 1 ~ 6:1.
2. the separation and refining method of producing ethylene from dehydration of ethanol according to claim 1, it is characterized in that the service temperature of ethylene rectification tower is-35 ~ 30.0 DEG C, working pressure is 1.3 ~ 4.5MPaG, and theoretical plate number is 50 ~ 140.
3. the separation and refining method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that ethylene rectification tower crude ethylene feed entrance point is at 40 ~ 110 theoretical tray places.
4. the separation and refining method of producing ethylene from dehydration of ethanol according to claim 1, it is characterized in that the service temperature of cut light tower is-45.0 ~-10.0 DEG C, working pressure is 1.2 ~ 4.3MPaG, and theoretical plate number is 2 ~ 60.
5. the separation and refining method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that heavy constituent stripping input of column position is at top.
6. the separation and refining method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that stripping overhead vapour phase returns the feed entrance point of ethylene rectification tower at 39 ~ 140 theoretical tray places.
7. the separation and refining method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that the part by weight of two strands of materials is 2 ~ 4:1.
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