CN104230623B - The energy-saving production method of producing ethylene from dehydration of ethanol - Google Patents
The energy-saving production method of producing ethylene from dehydration of ethanol Download PDFInfo
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- CN104230623B CN104230623B CN201310236945.9A CN201310236945A CN104230623B CN 104230623 B CN104230623 B CN 104230623B CN 201310236945 A CN201310236945 A CN 201310236945A CN 104230623 B CN104230623 B CN 104230623B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The present invention relates to the energy-saving production method of a kind of producing ethylene from dehydration of ethanol, mainly solve energy recovery in prior art insufficient, the organic wastewater of generation is not fully used, though or treated, there is complex process, long flow path, problem that investment is big.The present invention is comprised the following steps by employing: a) ethanol contacts with catalyst, generate the logistics 2 containing ethylene；B) logistics 2 obtains logistics 3 through heat reclaim unit recovery heat；Heat reclaim unit reclaims heat and produces steam stream 8；C) logistics 3 enters chilling tower, and with the washings counter current contacting entered from top, top obtains crude ethylene logistics 5, and bottom obtains organic wastewater logistics 6；D) logistics 6 enters stripping rectifying column middle and upper part, and tower top obtains logistics 9, and tower reactor obtains aqueous stream 7；E) logistics 8 be partially or wholly used for strip tower bottom of rectifying tower heating technical scheme preferably solve this problem, can be used in the commercial production of producing ethylene from dehydration of ethanol.
Description
Technical field
The present invention relates to the energy-saving production method of a kind of producing ethylene from dehydration of ethanol.
Background technology
Ethylene is a kind of important large organic chemical industry's base stock, is mainly used to produce the multiple Organic chemical products such as polyethylene, polrvinyl chloride, ethylene oxide/ethylene glycol, ethyl benzene/styrene, vinyl acetate.At present, domestic and international ethylene production mainly uses petroleum catalystic pyrolysis to produce.The research that non-petroleum feedstocks produced ethylene in recent years has new breakthrough, particularly producing ethylene by ethanol dehydration technology.This technology is with the ethanol deriving from biomass as raw material, so can avoid the dependence to petroleum resources.To the 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 ethylene, it is possible to resolve the difficult problem that fossil resource shortage is serious with environmental pollution.Especially with the fast development of biotechnology, the technology of biological legal system ethanol is the most perfect, and the source of raw material is increasingly extensive, and the cost of raw material is the most more rational so that producing ethylene from dehydration of ethanol technology attention.
Producing ethylene with ethyl alcohol, it is strong and have the technique of the market competitiveness that its key factor is to study a kind of new economy, and main goal in research is to improve technological process, reduces ethanol unit consumption, increases device benefit.
In the process 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 broadly divided into fixed-bed process and fluidized-bed process.ABB Lummu company once carried out ethanol dehydration reaction preparing ethylene (US4134926) in late nineteen seventies proposition fluidization, but this technology not yet obtains industrial applications.The predominantly fixed-bed process of commercial Application at present, including isothermal fixed-bed process and insulation fix bed technique.
Initial ethanol dehydration reaction is carried out in calandria type fixed bed, and reaction pressure is normal pressure, uses and directly heats or utilize the mode adding thermal medium (such as fused salt) heating indirectly to provide reaction heat for reaction.In course of reaction, reaction temperature and material flow are key factors, if temperature is the highest or material flow is the lowest, may result in the generation of other by-products, but if increasing flow velocity, the conversion ratio of ethanol can decline again.In order to solve this contradiction, United States Patent (USP) (US4232179) proposes skill in the thermal insulation of ethanol dehydration reaction, i.e. ethanol dehydration reaction is carried out in insulation fix bed, and reaction mass is heated to react temperature required before entering the reactor, to ensure being normally carried out of reaction.Afterwards, they also been proposed the insulation fix bed reaction process of syllogic (US4396789), and utilizes this technique to set up 60,000 tons/year of ethylene units in the early 1980s.This technique uses the insulation fix bed reactors of three series connection, preheats the ethanol of each Reactor inlet and steam charging with a stove, and the by-product such as unreacted ethanol and ether is carried out and circulated.The addition of steam decreases reaction coking, extends the life-span of catalyst, improves productivity.Plant running data show, when reactor inlet temperatures is 450 DEG C, ethanol conversion reaches 98%, catalyst regeneration cycle at least a year.Additionally Halcon/SD company develops the double mode technology of thermal insulation or isothermal fixed bed in nineteen seventies, and wherein isothermal bed technology has obtained industrial applications.Plant running data show: in reaction temperature 318 DEG C, 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 company develops again multistage insulation fixed bed reaction process: ethanol enters dehydration in multistage insulation fixed bed reaction after steam dilution and generates ethylene, reacting gas is scrubbed, compression, alkali cleaning and carry out cryogenic rectification more after drying, finally obtains polymer grade ethylene product.Examination data show: in reaction temperature 465 DEG C, liquid air speed (LHSV) 0. 8 hours-1And steam: ethanol than under conditions of for 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 uses shell and tube isothermal reactor, uses thermal oil system to provide the heat needed for reaction.The silicon one Al catalysts regeneration period is 3 weeks, often regenerates and once needs 3 days.Under the conditions of reaction temperature 315 DEG C, reaction pressure 0. 16MPa, ethylene selectivity about 94% (mole), ethanol conversion 99%.
In existing document or report, in particular how the recovery of heat energy and the problem of organic wastewater treatment process in shorter mention producing ethylene from dehydration of ethanol, reduce feed ethanol consumption and the energy-conservation technical problem of device.The sewage-treatment plant that the organic wastewater of commercial plant is directly entered outside device without process at present, on the one hand it is that the Organic substance in organic wastewater, particularly ethanol do not get utilization, ethanol consumption is made to increase, on the other hand it is because organic concentration in waste water higher, the difficulty making the sewage-treatment plant outside battery limit (BL) process sewage increases, and processing cost also increases.Patent CN101376551B proposes the organic wastewater used in the disposal methods producing ethylene from dehydration of ethanol of four cell process, there is complex process, long flow path, problem that investment is big.
Summary of the invention
The technical problem to be solved is that in prior art, producing ethylene from dehydration of ethanol energy recovery organic wastewater that is insufficient and that produce the most fully is processed, to reach the purpose of recycling, though or treated, there is complex process, long flow path, problem that investment is big, it is provided that the energy-saving production method of a kind of new producing ethylene from dehydration of ethanol.The method has that technique is simple, small investment and energy-conservation feature.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is as follows: the energy-saving production method of a kind of producing ethylene from dehydration of ethanol, comprises the following steps:
A) by vapour phase ethanol and γ-Al2O3, ZSM molecular sieve, at least one catalyst contact in molecular sieve or modenite, occur dehydration to generate the logistics 2 containing ethylene；
B) logistics 2 reclaims heat through heat reclaim unit, obtains temperature and is down to the logistics (3) of 110～350 DEG C), heat reclaim unit reclaims heat and produces steam stream 8；；
C) logistics 3 enters the bottom of chilling tower, carries out cooling washing with the washings counter current contacting entered from chilling top of tower, and the top of chilling tower obtains vapour phase crude ethylene logistics 5, and the bottom of chilling tower obtains containing ethanol, ether, the liquid phase organic wastewater logistics 6 of ethylene；
D) middle and upper part of logistics 6 entrance stripping rectifying column carries out stripping rectification, and tower top obtains containing ethanol, ether, the logistics 9 of ethylene, and tower reactor obtains aqueous stream 7, content of organics≤20ppm in logistics 7；
E) logistics 8 is as thermal source, is partially or wholly used for stripping the heating of tower bottom of rectifying tower.
In technique scheme, it is preferable that it is calandria type fixed bed, multistage insulation fixed bed or single stage adiabatic fixed bed that ethanol dehydration reaction produces the reactor of ethylene.
In technique scheme, it is preferable that the reaction temperature of ethanol dehydration is 300～510 DEG C, reaction pressure is calculated as 0.01～5.0MPaG with gauge pressure, and reaction weight space velocity is 0.1～10 hour-1。
In technique scheme, it is preferable that described chilling tower is packed tower, plate column or void tower.
In technique scheme, it is preferable that the operation temperature of chilling tower is 30～120 DEG C, operation pressure is calculated as 0.01～4.5MPaG with gauge pressure, and liquid gas weight ratio is 1.2～30, and theoretical cam curve is 2～18.
In technique scheme, it is preferable that the operation temperature of stripping rectifying column is 30～210. 0 DEG C, operation pressure is 0～1.0MPaG, and theoretical cam curve is 2～98, and the feed entrance point of organic wastewater is at 1～85 theoretical trays.
In technique scheme, it is preferable that described heat reclaim unit is waste heat boiler.
In technique scheme, it is preferable that the logistics 9 of stripping rectifying column tower top is vapour phase or liquid phase extraction.
In technique scheme, it is preferable that when logistics 9 is vapour phase extraction, organic wastewater logistics 6 feed entrance point is at first block of the top column plate of stripping rectifying column.
In technique scheme, it is preferable that when logistics 9 is liquid phase extraction, the reflux ratio of stripping rectifying column is 0.1～6.
In the inventive method, the heat that heat reclaim unit reclaims is used for stripping tower bottom of rectifying tower heating.If this partial heat is inadequate, also can be directly entered the bottom of tower as thermal source being passed through steam at the bottom of stripping rectifying tower, it is also possible to use steam, deep fat, electricity etc. to provide thermal source with the form of reboiler or heater for stripping rectifying column.
In the present invention, the reacting gas heat owing to being reclaimed by heat reclaim unit is used as to strip the thermal source of rectifying column, and use the organic wastewater produced in stripping rectifying column PROCESS FOR TREATMENT producing ethylene from dehydration of ethanol, ethanol, ether, ethylene, carbon three and the Organic substance of above hydrocarbon thereof in removing organic wastewater, plant energy consumption decreases, Organic substance, particularly ethanol in organic wastewater get utilization, and reduce the consumption of feed ethanol.Use the inventive method, have that technique is simple, flow process is short, energy consumption is low and the feature of small investment, device for ton, coarse ethanol 222 tons/year (concentration is about 80 weight %) in recyclable organic wastewater, in organic wastewater, organic concentration is down to trace from 0.265 weight %, reclaims heat energy 44.776kw, equivalent minimizing steam 605 tons/year, reduce chilling tower recirculated cooling water 234679 tons/year, achieve preferable technique effect.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
In Fig. 1,1 is raw material vapour phase ethanol, 2 reacting gas generated for dehydration, 3 is the reacting gas after recovery heat, and 4 is the washings of chilling tower, and 5 is the crude ethylene gas after chilling washs, 6 is the organic wastewater after chilling washing, and 7 is treated lean organic wastewater, and 8 is the steam that waste heat boiler occurs, the tower top material that 9 is stripping rectifying column, 10 is boiler feedwater, and 1a is reactor, and 2a is waste heat boiler, 3a is chilling tower, and 4a is stripping rectifying column.
In Fig. 1, raw material vapour phase ethanol enters gas solid phase fixed bed reactor 1a, and containing γ-Al2O3, ZSM molecular sieve, one or more catalyst contact of molecular sieve or modenite, dehydration produces ethylene and other by-product stream 2.Reacting gas 2 is after waste heat boiler 2a reclaims heat, enter gas chilled tower 3a, with washings 4 chilling washing reaction gas, obtaining crude ethylene 5 after chilling washing goes follow up device to process, organic wastewater 6 after chilling washing enters stripping rectifying column 4a, isolate the logistics 9 containing ethanol, ether and ethylene, carbon three and above hydrocarbon thereof at tower top, discharge aqueous stream 7 in tower reactor.Logistics 9 can be vapour phase extraction, it is also possible to be or liquid phase extraction.When logistics 9 is vapour phase extraction, organic wastewater logistics 6 feed entrance point is at the column plate of first block of rectifying column top of stripping.When logistics 9 is liquid phase extraction, reflux ratio is 0.1～6.
Below by embodiment, the present invention is further elaborated.
Detailed description of the invention
[embodiment 1]
Technical scheme as shown in Figure 1, raw material vapour phase ethanol is in reaction temperature 345 DEG C, reaction pressure 0.06MPaG, liquid phase ethanol air speed 0.9hr-1Under conditions of, with γ-Al2O3Catalyst contact dehydration produces ethylene, reacting gas is after waste heat boiler reclaims heat, temperature is down to 160 DEG C and is entered chilling tower, wash with washings under conditions of top pressure 0.04MPaG, top temperature 40 DEG C, liquid phase organic wastewater after washing enters stripping rectifying column and separates, separate containing organic secondary organic wastewater at tower top, isolate the lean organic wastewater containing micro-content organism in tower reactor.The each composition flow rate of organic wastewater is: carbon dioxide 0.016 kg/hr, ethylene 0.799 kg/hr, 0.002 kg/hr of ethane, 0.001 kg/hr of propane, 0.977 kg/hr of acetaldehyde, ethanol 22.229 kgs/hr, ether 0.398 kg/hr, heavy constituent 0.07 kg/hr, 9204.193 kgs/hr of water.The stripping lean organic wastewater of tower bottom of rectifying tower is 9200 kgs/hr, and wherein Organic substance is 4ppm.Stripping rectifying column overhead vapor phase enters condenser, flow is 103.596 kgs/hr, strips rectifier column reflux 74.910 kgs/hr, strips rectifying column extraction richness organic wastewater 27.744 kgs/hr, concentration of alcohol 79.6%wt, strips rectifying tower top gas phase 0.942 kg/hr.The tower top temperature of stripping rectifying column is 90.8 DEG C, and pressure is 0.11MPaG, and bottom temperature is 125 DEG C, full tower theoretical cam curve is 12, feed entrance point is at middle part, and the heat that waste heat boiler reclaims is completely used for stripping tower bottom of rectifying tower heating, and the form with reboiler provides thermal source for stripping rectifying column the most again.
Waste heat boiler reclaims heat energy 44.776kw, and the thermic load of stripping distillation column reboiler is 578.635kw, annual saving low-pressure steam 605 tons；Reduce chilling tower cooler load 35.7kw, save recirculated cooling water 234679 tons/year the equivalent whole year.
[embodiment 2]
Same embodiment [embodiment 1], only changes the theoretical stage of stripping rectifying column: full tower theoretical cam curve is 22, and feed entrance point is in middle and upper part.The stripping lean organic wastewater of tower bottom of rectifying tower is 9200 kgs/hr, and wherein Organic substance is 3ppm.Stripping rectifying column overhead vapor phase enters condenser, flow is 40.577 kgs/hr, strips rectifier column reflux 11.890 kgs/hr, strips rectifying column extraction richness organic wastewater 27.744 kgs/hr, concentration of alcohol 79.6%wt, strips rectifying tower top gas phase 0.942 kg/hr.The tower top temperature of stripping rectifying column is 90.8 DEG C, and pressure is 0.11MPaG, and bottom temperature is 125 DEG C.
Reacting gas temperature is down to 160 DEG C through waste heat boiler, reclaims heat and is completely used for stripping tower bottom of rectifying tower heating, and the form with reboiler provides thermal source for stripping rectifying column the most again.
Waste heat boiler reclaims heat energy 44.776kw, and the thermic load of stripping distillation column reboiler is 557.833kw, annual saving low-pressure steam 605 tons；Reduce chilling tower cooler load 35.7kw, save recirculated cooling water 234679 tons/year the equivalent whole year.
[embodiment 3]
With [embodiment 1], only changing the tower reactor mode of heating of stripping distillation column, the bottom being directly entered tower with steam replaces reboiler, tower top frozen-free device, and vapour phase extraction returns producing ethylene from dehydration of ethanol device.Organic wastewater logistics 6 feed entrance point is at first block of the top column plate of stripping rectifying column.The stripping lean organic wastewater of tower bottom of rectifying tower is 10538.662 kgs/hr, and wherein Organic substance is 12.7ppm.Stripping rectifying column overhead vapor phase (rich organic wastewater) flow is 240.024 kgs/hr, concentration of alcohol 9.23%wt.The tower top temperature of stripping rectifying column is 120.5 DEG C, and pressure is 0.11MPaG, and bottom temperature is 123.3 DEG C.
Reacting gas temperature is down to 160 DEG C through waste heat boiler, reclaims heat and is completely used for stripping tower bottom of rectifying tower heating, provides thermal source with the form that steam is directly entered for stripping rectifying column the most again.
Waste heat boiler reclaims heat energy 44.776kw, and the flow of stripping distillation column stripped vapor is 11795 tons/year.Annual saving low-pressure steam 605 tons；Reduce chilling tower cooler load 35.7kw, save recirculated cooling water 234679 tons/year the equivalent whole year.
Claims (9)
1. an energy-saving production method for producing ethylene from dehydration of ethanol, comprises the following steps:
A) by vapour phase ethanol and γ-Al2O3, ZSM molecular sieve, in beta-molecular sieve or modenite extremely
Few a kind of catalyst contact, occurs dehydration to generate the logistics (2) containing ethylene；
B) logistics (2) reclaims heat through heat reclaim unit, obtains temperature and is down to 110～350 DEG C
Logistics (3), heat reclaim unit reclaim heat produce steam stream (8)；
C) logistics (3) enters the bottom of chilling tower, connects with the washings adverse current entered from chilling top of tower
Touching and carry out cooling washing, the top of chilling tower obtains vapour phase crude ethylene logistics (5), the bottom of chilling tower
Obtain containing ethanol, ether, liquid phase organic wastewater logistics (6) of ethylene；
D) logistics (6) enter stripping rectifying column middle and upper part carry out strip rectification, tower top obtain containing ethanol,
Ether, the logistics (9) of ethylene, tower reactor obtains aqueous stream (7), content of organics in logistics (7)
≤20ppm；
E) logistics (8), as thermal source, is partially or wholly used for stripping the heating of tower bottom of rectifying tower；
Wherein, the operation temperature of described stripping rectifying column is 30～210.0 DEG C, operation pressure be 0～
1.0MPaG, theoretical cam curve is 2～98, and the feed entrance point of organic wastewater is at 1～85 theoretical trays
Place.
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
It is calandria type fixed bed, multistage insulation fixed bed for being that ethanol dehydration reaction produces the reactor of ethylene
Or single stage adiabatic fixed bed.
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
The reaction temperature being ethanol dehydration is 300～510 DEG C, reaction pressure with gauge pressure be calculated as 0.01～
5.0MPaG, reaction weight space velocity is 0.1～10 hour-1。
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
It is that described chilling tower is packed tower, plate column or void tower.
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
The operation temperature being chilling tower is 30～120 DEG C, operation pressure with gauge pressure be calculated as 0.01～
4.5MPaG, liquid gas weight ratio is 1.2～30, and theoretical cam curve is 2～18.
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
It is that described heat reclaim unit is waste heat boiler.
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
It is that the logistics (9) stripping rectifying column tower top is vapour phase or liquid phase extraction.
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
Being when logistics (9) is vapour phase extraction, organic wastewater logistics (6) feed entrance point is at stripping rectifying column
At the column plate of first block of top.
The most energy-saving production method of producing ethylene from dehydration of ethanol, its feature
Being when logistics (9) is liquid phase extraction, the reflux ratio of stripping rectifying column is 0.1～6.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4134926A (en) * | 1977-04-18 | 1979-01-16 | The Lummus Company | Production of ethylene from ethanol |
| CN101376551A (en) * | 2007-08-31 | 2009-03-04 | 中国石油化工股份有限公司 | Method for processing process waste water of ethylene preparation by ethanol dehydration |
| CN102372567A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for producing ethene by ethanol dehydration |
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2013
- 2013-06-17 CN CN201310236945.9A patent/CN104230623B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4134926A (en) * | 1977-04-18 | 1979-01-16 | The Lummus Company | Production of ethylene from ethanol |
| CN101376551A (en) * | 2007-08-31 | 2009-03-04 | 中国石油化工股份有限公司 | Method for processing process waste water of ethylene preparation by ethanol dehydration |
| CN102372567A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for producing ethene by ethanol dehydration |
Non-Patent Citations (1)
| Title |
|---|
| 乙醇脱水制取乙烯的工业生产;徐晓育等;《日用化学工业》;19881231;第23卷(第5期);第247-252页 * |
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