CN103664448B - Wood-based composites are dehydrated the separation and refining method of ethene processed - Google Patents
Wood-based composites are dehydrated the separation and refining method of ethene processed Download PDFInfo
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- CN103664448B CN103664448B CN201210324400.9A CN201210324400A CN103664448B CN 103664448 B CN103664448 B CN 103664448B CN 201210324400 A CN201210324400 A CN 201210324400A CN 103664448 B CN103664448 B CN 103664448B
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Abstract
The present invention relates to the separation and refining method that a kind of wood-based composites are dehydrated ethene processed, the ethene for mainly solving the problems, such as to be not directed in previous literature is dehydrated the separating technology of product in ethene processed and how to improve yield of ethene, particularly reclaims the technical problem of light component stream and the ethene in heavy constituent material.Technical scheme of the invention by using three-column process flow, ethylene rectifying column tower reactor isolate heavy constituent containing ethene, and at the top of stripping destilling tower, tower top isolates the ethene containing light component, delivers to the middle part of lights column；Strip the middle and lower part that overhead vapour phase returns to ethylene rectifying column, bottom of towe discharge heavy constituent；The overhead stream of light component rectifying column is after partial condensation, liquid-phase reflux, is arranged outside gas phase, tower reactor obtains the technical scheme of ethylene product, preferably solves the problem, available in producing ethylene from dehydration of ethanol industrial production.
Description
Technical field
The present invention relates to the separation and refining method that a kind of wood-based composites are dehydrated ethene processed.
Background technology
Ethene is a kind of important large organic chemical industry's base stock, is mainly used to produce polyethylene, polyvinyl chloride, epoxy
A variety of Organic chemical products such as ethane/ethylene glycol, ethyl benzene/styrene, vinyl acetate.At present, domestic and international ethylene production master
Petroleum catalystic pyrolysis is used to produce.The research for producing ethene to non-petroleum feedstocks in recent years has new breakthrough, especially
It is producing ethylene by ethanol dehydration technology.The technology is using the ethanol from agricultural byproducts as raw material, can so be avoided to oil
The dependence of resource.To oil-poor and national and regional based on agricultural, the raw material for producing ethanol is easy to get and guaranteed, to produce second
Alkene has established enough raw material bases, can solve fossil resource shortage and the serious problem of environmental pollution.
Producing ethylene with ethyl alcohol, its key factor are to study a kind of strong and with the market competitiveness the technique of new economy,
Main goal in research is modified technique flow, reduces ethanol unit consumption, increases device benefit.
In the process of producing ethylene from dehydration of ethanol, at home and abroad many of document or patent disclosed in oneself warp are square
Method, its basic technology are broadly divided into fixed-bed process and fluidized-bed process.ABB Lummu:Company once proposed in late nineteen seventies
Ethanol dehydration reaction preparing ethylene (USP4134926) is carried out with fluidization, but this technology not yet obtains industrialization and answered
With.The predominantly fixed-bed process, including isothermal fixed-bed process and insulation fix bed technique of commercial Application at present.
For initial ethanol dehydration reaction in calandria type fixed bed middle progress, reaction pressure is normal pressure, using directly heating or
Person provides reaction heat using the mode for heating medium (such as fused salt) indirectly heat for reaction.During the course of the reaction, reaction temperature with
Material flow is key factor, if temperature is too high or material flow is too low, may result in the generation of other accessory substances, still
If increasing flow velocity, the conversion ratio of ethanol can drop to again solves this contradiction, and United States Patent (USP) (USP4232179) proposes
Skill in the thermal insulation of ethanol dehydration reaction, i.e. ethanol dehydration reaction are in insulation fix bed middle progress, and reaction mass is into reactor
Before be heated to react required temperature, with ensure reaction be normally carried out.Afterwards, it is insulation fix bed anti-to have also been proposed three-stage for they
Technique (USP4396789) is answered, and 60,000 tons/year of ethylene units are established using the technique in the early 1980s.The work
Skill uses the insulation fix bed reactor of three series connection, and the ethanol of each Reactor inlet and steam are preheated with a stove
Mixed feeding, the accessory substance such as unreacted ethanol and ether carry out circulation.The addition of steam reduces reaction coking, extends catalysis
In the life-span of agent, improve yield.Plant running as shown by data, when reactor inlet temperatures are 450 DEG C, ethanol conversion reaches
98, catalyst regeneration cycle at least 1 year.Other Halcon/SD companies and tenth century the seventies develop adiabatic or isothermal
The double mode technology of fixed bed, wherein isothermal bed technology have obtained industrial applications.Plant running as shown by data：Reacting
318 DEG C of temperature, liquid air speed (LHSV) 0.23 hour-1Under conditions of, ethylene selectivity 96.8% (mole), ethanol conversion
99.1%, catalyst regeneration cycle 8 months.After, Halcon/SD companies develop multistage insulation fixed bed reaction process again：Second
Alcohol enters dehydration generation ethene in multistage insulation fixed bed reaction after steam dilution, and reacting gas is scrubbed, compresses, alkali cleaning
With cryogenic rectification is carried out after drying again, finally obtain polymer grade ethylene product.Try as shown by data：In 465 DEG C of reaction temperature, liquid
Body air speed (LHSV) 0.8 hour-1And steam：Ethanol ratio is 3：Under conditions of 1, ethylene selectivity 99.4% (mole), ethanol turns
Rate 99.9%, catalyst regeneration cycle 8 months.Lummus companies realize fixed-bed process early in nineteen sixties
Industrialization.The technique uses shell and tube isothermal reactor, and the heat needed for reaction is provided using thermal oil system.The aluminium of silicon one is urged
The agent regeneration period is 3 weeks, and often regenerating once needs 3 days.Under the conditions of 315 DEG C of reaction temperature, reaction pressure 0.16MPa, ethene
About 94% (mole) of selectivity, ethanol conversion 99%.
In existing literature or report, shorter mention ethene is dehydrated the separating technology of product in ethene processed and how to improve ethene
The problem of yield, particularly reclaim the technical problem of light component stream and the ethene in heavy constituent material.Commercial plant at present
Separating technology is to use two-tower process, and crude ethylene is introduced into ethylene rectifying column, and tower top light component is arranged after partial condensation outside gas phase,
Liquid phase delivers to light component stripper, the light component in liquid phase is removed, to obtain 99.99% smart ethene.The technique, though it can obtain
99.99% smart ethene, but due to removing light component using the technique of stripping destilling tower, and the second in heavy constituent logistics is not reclaimed
Alkene, the problem of ethylene loss be present.Patent (ZL200710040705.64) proposes the method using adiabatic flash, reclaims ethene
Ethene in rectifying column kettle liquid, though recyclable part ethene, organic efficiency be not high.The present invention provides a kind of new one kind biology
The separation and purification technique of matter producing ethylene from dehydration of ethanol, this method have that ethylene recovery efficiency is high, energy consumption is low, good product quality spy
Point.
The content of the invention
The technical problems to be solved by the invention are that the separation of product in producing ethylene from dehydration of ethanol is not directed in previous literature
Technological problemses, in particular how improve yield of ethene, reduce the technical problem of energy consumption, there is provided a kind of new wood-based composites dehydration
The separation and refining method of ethene processed.The advantages of this method has the high income of ethene, and energy consumption is low.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is as follows：A kind of wood-based composites are dehydrated second processed
The separation and purification technique of alkene, mixture and light component containing ethene, ethane and carbon three and its above hydrocarbon enter ethylene rectifying column,
Tower top isolates the ethene containing light component, partial reflux after vapour phase is condensed, partly to light component rectifying column middle part, is arranged in tower reactor
Go out the heavy constituent containing ethene；Heavy constituent containing ethene enters the top of heavy constituent stripping destilling tower, after stripping separated, tower
The middle and lower part that vapour phase returns to ethylene rectifying column is pushed up, tower reactor is heavy constituent, outer row；Liquid phase ethylene containing light component is through light component rectifying
After tower separation, overhead vapor phase is condensed to separate vapour phase light component, and outer row, condensate liquid returns to cut light tower as backflow, light
The bottom of component rectifying column obtains liquid phase ethylene product.
In above-mentioned technical proposal, the operation temperature of ethylene rectifying column is -35~30.0 DEG C, preferred scope is -30~
25.0℃；Operating pressure is 1.3~4.5MPaG, and preferred scope is 1.5~4MPaG；Theoretical cam curve is 50~140, preferably model
Enclose for 60~120；Feed entrance point is at 40~110 theoretical trays, and preferred scope is at 60~100 theoretical trays.Light component essence
The operation temperature for evaporating tower is -35~10.0 DEG C, and preferred scope is -40.0~-8.0 DEG C；Operating pressure be 1.2~
4.5MPaG, preferred scope are 1.5~4.0MPaG；Theoretical cam curve is 2~60, and preferred scope is 5~55；Feed entrance point is 2
At~58 theoretical trays, preferred scope is at 5~50 theoretical trays.Ethylene rectifying column tower top liquid phase is divided into two strands of materials：Ethene
The backflow of rectifying column and the charging of light component rectifying column, the ratio of two strands of materials is 1~6, and preferred scope is 2~4.5.Heavy constituent
The operation temperature for stripping destilling tower is -15~80 0 DEG C, and preferred scope is -10~70 0 DEG C；Operating pressure be 1.0~
4.0MPaG, preferred scope are 1.5~3.0MPaG；Theoretical cam curve is 2~50, and preferred scope is 5~40；Feed entrance point is pushing up
Portion.Strip overhead vapour phase and return to the feed entrance point preferred scope of ethylene rectifying column at 39~140 theoretical trays.This hair
Light component described in bright is primarily referred to as hydrogen, methane, carbon monoxide.
Due to being carried out using ethylene rectifying column, light component rectifying column and heavy constituent stripping destilling tower to crude ethylene in the present invention
Separation and purification, heavy constituent and light component in ethene are removed, avoids ethylene component more in former technique in lightness-removing column and second
Circulated between alkene rectifying column, improve the yield of ethene, reduce energy consumption；On the other hand can allow in ethylene distillation tower bottoms
Ethylene contents greatly increase, and are more prone to ethylene rectifying column operation.Tests prove that using technical scheme, thick second
Alkene separating energy consumption reduces by 13.25%, and ethylene product purity is further enhanced, and the ethylene volume remained in heavy constituent drops from 22%
As little as 3%, ethylene product purity and yield are further enhanced, and achieve preferable technique effect.
Brief description of the drawings
Fig. 1 is the schematic flow sheet for the separation and purification technique that wood-based composites of the present invention are dehydrated ethene processed.
In Fig. 1,1 is the crude ethylene from ethene drying system, and 2 be the tower reactor containing finite concentration Ethylene vinyl rectifying column
Heavy constituent, 3 be the tower top material of ethylene rectifying column, and 4 be stripping overhead vapor phase stream, and 5 be ethylene product, and 6 be ethene
The backflow of rectifying column, 7 be the charging of light component rectifying column, and 8 be the tower top material of light component rectifying column, and 9 be light component rectifying column
Outer row's light component, 10 be the backflow of light component rectifying column, and 11 be stripping destilling tower tower reactor heavy constituent, and 1a is ethylene rectifying column, 2a
For the condenser of ethylene rectifying column, 3a is light component rectifying column, and 4a is that heavy constituent strips destilling tower, and 5a is light component rectifying column
Condenser, 6a are the return tank of light component rectifying column.
Below by embodiment, the present invention is further elaborated.
Embodiment
【Embodiment 1】
Crude ethylene from ethene drying system is separated into ethylene rectifying column, is separated in tower top containing light component
Ethene, heavy constituent is isolated in tower reactor.Crude ethylene each group shunt volume is：0.070 kg/hr of hydrogen, 0.070 kilogram of methane/
Hour, 0.557 kg/hr of carbon monoxide, 1274.518 kgs/hr of ethene, 7.060 kgs/hr of ethane, propane
1.555 kgs/hr, 0.113 kg/hr of acetaldehyde, 5.631 kgs/hr of ether, 33.957 kgs/hr of heavy constituent.
The restructuring of ethylene rectifying column tower reactor is divided into 83.866 kgs/hr, and wherein ethene is 18.593 kgs/hr, ethene
Rectifying column tower top light component is 4712.040 kgs/hr, and wherein ethene is 4709.413 kgs/hr, after condensed, is divided into
Two strands, the backflow of ethylene rectifying column is 3438.507 kgs/hr, the charging of light component rectifying column for 1273.520 kilograms/it is small
When, outer row's light component is zero.The tower top temperature of ethylene rectifying column is -25.0 DEG C, pressure 2.15MPaG, bottom temperature 9.3
DEG C, full tower theoretical cam curve is 80, and feed entrance point is in middle and lower part.The thermic load of ethylene rectifying column condenser is 434.501kw.This
Light component described in invention is primarily referred to as hydrogen, methane, carbon monoxide.
Ethylene rectifying column tower reactor restructuring lease making pump pressure, which is delivered at the top of stripping destilling tower, carries out stripping distillation, strips destilling tower
Tower top temperature be 9.6 DEG C, pressure 2.16MPaG, bottom temperature be 59 DEG C, full tower theoretical cam curve be 12；Distilled through stripping
Afterwards, tower top steams the mainly Matter Transfer containing ethene and enters ethylene rectifying column bottom, and flow is 33.866 kgs/hr, tower bottom
Discharge mainly contains ethane and C3 +Mixture, flow is 50.102 kgs/hr, wherein containing 1.696 kgs/hr of ethene.Vapour
The thermic load for carrying destilling tower reboiler is 4.691kw.
The tower top temperature of light component rectifying column is -22.7 DEG C, pressure 2.35MPaG, and bottom temperature is -21.6 DEG C, full tower
Theoretical cam curve is 18, and feed entrance point is in middle and upper part.After distillation, it is cold through part that tower top steams the light component material containing ethene
Solidifying, vapor-liquid separation, liquid phase return to light component rectifying column as backflow, arranged outside gas phase, flow is 7.815 kgs/hr, wherein containing
Ethene is 7.133 kgs/hr.The bottom of light component rectifying column produces smart ethylene product, and flow is 1265.638 kilograms/it is small
When, Ethylene purity reaches 99.998%.The condenser heat load of light component rectifying column is 29.141kw, and the thermic load of reboiler is
41.149kw。
Separating technology yield of ethene is 99.30% (weight).
【Embodiment 2】
Together【Embodiment 1】, the theoretical stage of a change ethylene rectifying column：Full tower theoretical cam curve is 92, and feed entrance point exists
Middle and lower part, Qi Tatong【Embodiment 1】.
The restructuring of ethylene rectifying column tower reactor is divided into 83.939 kgs/hr, and wherein ethene is 18.609 kgs/hr, ethene
Rectifying column top return is 3438.539 kgs/hr, and the charging of light component rectifying column is 1273.531 kgs/hr.Ethene
The tower top temperature of rectifying column is -25.0 DEG C, pressure 2.15MPaG, and bottom temperature is 9.3 DEG C.The heat of ethylene rectifying column condenser
Load is 434.503kw.
The tower top temperature for stripping destilling tower is 9.6 DEG C, pressure 2.16MPaG, and bottom temperature is 59 DEG C, and tower top steams master
The Matter Transfer for containing ethene enters ethylene rectifying column bottom, and flow is 33.937 kgs/hr, and tower bottom discharge mainly contains ethane
And C3 +Mixture, flow is 50.102 kgs/hr, wherein containing 1.688 kgs/hr of ethene.Strip destilling tower reboiler
Thermic load be 4.699kw.
The tower top temperature of light component rectifying column is -22.7 DEG C, pressure 2.35MPaG, and bottom temperature is -21.6 DEG C, tower top
Gas phase effluent stream amount is 7.819 kgs/hr, wherein being 7.136 kgs/hr containing ethene.Adopt the bottom of light component rectifying column
Go out smart ethylene product, flow is 1265.713 kgs/hr, and Ethylene purity reaches 99.998%.The condenser of light component rectifying column
Thermic load is 29.139kw, and the thermic load of reboiler is 41.152kw.
Separating technology yield of ethene is 99.31% (weight).
【Embodiment 3】
Together【Embodiment 1】, the theoretical stage of a change light component rectifying column：Full tower theoretical cam curve is 25, feed entrance point
In middle and upper part, Qi Tatong【Embodiment 1】.
The restructuring of ethylene rectifying column tower reactor is divided into 83.871 kgs/hr, and wherein ethene is 18.594 kgs/hr, ethene
Rectifying column top return is 3438.540 kgs/hr, and the charging of light component rectifying column is 1273.531 kgs/hr.Ethene
The tower top temperature of rectifying column is -25.0 DEG C, pressure 2.15MPaG, and bottom temperature is 9.3 DEG C.The heat of ethylene rectifying column condenser
Load is 434.504kw.
The tower top temperature for stripping destilling tower is 9.6 DEG C, pressure 2.16MPaG, and bottom temperature is 59 DEG C, and tower top steams master
The Matter Transfer for containing ethene enters ethylene rectifying column bottom, and flow is 33.872 kgs/hr, and tower bottom discharge mainly contains ethane
And C3 +Mixture, flow is 50.9 kgs/hr, wherein containing 1.695 kgs/hr of ethene.Strip destilling tower reboiler
Thermic load is 4.692kw.
The tower top temperature of light component rectifying column is -22.7 DEG C, pressure 2.35MPaG, and bottom temperature is -21.6 DEG C, tower top
Gas phase effluent stream amount is 7.833 kgs/hr, wherein being 7.148 kgs/hr containing ethene.Adopt the bottom of light component rectifying column
Go out smart ethylene product, flow is 1265.783 kgs/hr, and Ethylene purity reaches 99.998%.The condenser of light component rectifying column
Thermic load is 29.131kw, and the thermic load of reboiler is 41.152kw.
Separating technology yield of ethene is 99.31% (weight).
【Comparative example 1】
Crude ethylene from ethene drying system is separated into ethylene rectifying column, is separated in tower top containing light component
Ethene, heavy constituent is isolated in tower reactor.Crude ethylene each group shunt volume is same as above, and the restructuring of ethylene rectifying column tower reactor is divided into 62.082 thousand
Grams Per Hour, wherein ethene are 13.765 kgs/hr.Ethylene distillation column overhead light component is 5510.374 kgs/hr, its
Middle ethene is 5502.95 kgs/hr, after condensed, is divided into two strands, the backflow of ethylene rectifying column for 4248.924 kilograms/it is small
When, the charging of light component stripper is 1573.673 kgs/hr.The tower top temperature of light component stripper is -22.4 DEG C, pressure
For 2.35MPaG, bottom temperature is -21.6 DEG C, and full tower theoretical cam curve is 18, and feed entrance point is at top.After stripping, tower top
The light component material containing ethene is steamed to mix with the uncooled light component material of ethylene rectifying column, through partial condensation, vapor-liquid separation,
Liquid phase mixes with the overhead condensation liquid of ethylene rectifying column, is arranged outside gas phase, and flow is 11.422 kgs/hr, wherein being containing ethene
10.763 kgs/hr.The bottom of light component stripper produces smart ethylene product, and flow is 1250.053 kgs/hr, ethene
Purity reaches 99.996%.The condenser heat load of ethylene rectifying column is 507.888kw, and the thermic load of light component condenser is
28.712kw, separating technology yield of ethene are 98.08% (weight).
【Comparative example 2】
Crude ethylene from ethene drying system is separated into ethylene rectifying column, is separated in tower top containing light component
Ethene, heavy constituent is isolated in tower reactor.Crude ethylene each group shunt volume is same as above.Ethylene rectifying column tower reactor restructuring lease making pump pressure, heating
Deliver to adiabatic flash tank.Flash drum overhead gas phase returns to ethylene distillation tower bottom, flash tank bottom extraction liquid phase heavy constituent, each group
Shunt volume is：4.415 kgs/hr of ethene, 7.068 kgs/hr of ethane, 1.555 kgs/hr of propane, acetaldehyde 0.113 thousand
Grams Per Hour, 5.630 kgs/hr of ether, 33.956 kgs/hr of heavy constituent.The thermic load of heater is 10.864kw, second
Alkene yield is 98.80% (weight).
Claims (5)
- It is mixed containing ethene, ethane and carbon three and its above hydrocarbon 1. a kind of wood-based composites are dehydrated the separation and refining method of ethene processed Compound and light component enter ethylene rectifying column, and the ethene containing light component, partial reflux after vapour phase is condensed, portion are isolated in tower top Divide in the middle part of light component rectifying column, the heavy constituent containing ethene is discharged in tower reactor；Heavy constituent containing ethene enters heavy constituent stripping and steamed The top of tower is evaporated, after stripping separated, overhead vapor phase returns to the middle and lower part of ethylene rectifying column, and tower reactor is heavy constituent, outer row； For liquid phase ethylene containing light component after the separation of light component rectifying column, overhead vapor phase is condensed to separate vapour phase light component, outer row, condensation Liquid returns to light component rectifying column as backflow, and liquid phase ethylene product is obtained in the bottom of light component rectifying column；Wherein, the operation temperature of the ethylene rectifying column is -30~25.0 DEG C, and operating pressure is 1.5~4MPaG, and is not 2.15MPaG, theoretical cam curve are 60~120, and feed entrance point is at 60~100 theoretical trays；The ethylene rectifying column tower top liquid phase is divided into two strands of materials：The backflow of ethylene rectifying column and the charging of light component rectifying column, The backflow of the ethylene rectifying column is 3438.507 kgs/hr, the charging of the light component rectifying column for 1273.520 kilograms/ Hour, or the ethylene rectifying column overhead reflux is 3438.539 kgs/hr, the charging of the light component rectifying column is 1273.531 kgs/hr, or the ethylene rectifying column overhead reflux is 3438.540 kgs/hr, the light component rectifying The charging of tower is 1273.531 kgs/hr；The operation temperature of the heavy constituent stripping destilling tower is -15~59 DEG C, operating pressure 2.16MPaG, theoretical cam curve For 12, feed entrance point is at top.
- 2. wood-based composites are dehydrated the separation and refining method of ethene processed according to claim 1, it is characterised in that light component essence The operation temperature for evaporating tower is -45.0~-10.0 DEG C, and operating pressure is 1.2~4.3MPaG, and theoretical cam curve is 2~60, is entered Discharge position is at 2~58 theoretical trays.
- 3. wood-based composites are dehydrated the separation and refining method of ethene processed according to claim 2, it is characterised in that light component essence The operation temperature for evaporating tower is -40.0~-8.0 DEG C, and operating pressure is 1.5~4.0MPaG, and theoretical cam curve is 5~55, charging Position is at 5~50 theoretical trays.
- 4. wood-based composites are dehydrated the separation and refining method of ethene processed according to claim 1, it is characterised in that heavy constituent vapour The operation temperature for carrying destilling tower is -10~59 DEG C.
- 5. wood-based composites are dehydrated the separation and refining method of ethene processed according to claim 1, it is characterised in that stripping distillation Column overhead vapour phase returns to the feed entrance point of ethylene rectifying column at 39~120 theoretical trays.
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| 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 |
| CN101973831A (en) * | 2010-10-14 | 2011-02-16 | 东华工程科技股份有限公司 | Separation method for producing light olefins from oxygenated chemicals |
| CN103420752A (en) * | 2012-05-16 | 2013-12-04 | 中国石油化工股份有限公司 | Separation refinement method for ethylene preparation through biomass ethanol dehydration |
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| 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 |
| CN101973831A (en) * | 2010-10-14 | 2011-02-16 | 东华工程科技股份有限公司 | Separation method for producing light olefins from oxygenated chemicals |
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