CN104230623A - Energy-efficient method for ethylene production from ethanol dehydration - Google Patents
Energy-efficient method for ethylene production from ethanol dehydration Download PDFInfo
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Abstract
The invention relates to an energy-efficient method for ethylene production from ethanol dehydration, and mainly solves the problems in the prior art that recovery of heat energy is incomplete, utilization of produced organic wastewater is incomplete, or that the organic wastewater is treated, but the process is complex, long in flow and large in investment. The method comprises the following steps: a) contacting ethanol with a catalyst to generate a material flow 2 containing ethylene; b) recovering heat in the material flow 2 by a heat recovery device to obtain a material flow 3; and generating a steam material flow 8 by the heat recovered by the heat recovery device; c) introducing the material flow 3 into the a quench tower to conduct counter current contact with washing water entering from the top, so as to obtain a coarse ethylene material flow 5 in the top and an organic wastewater material flow 6 at the bottom; d) introducing the material flow 6 into the upper middle part of a stripping rectification tower to obtain a material flow 9 at the tower top and a material flow 7 containing water at the tower bottom; and e) using part or all of the material flow 8 to heat tower bottom of the stripping rectification tower bottom. The technical scheme well solves the above problems and can be used in industrial production for preparing ethylene by ethanol dehydration.
Description
Technical field
The present invention relates to a kind of energy-saving production 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 biomass 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.Especially along with the fast development of biotechnology, the technology of biological legal system ethanol is constantly perfect, and the source of raw material is increasingly extensive, and the cost of raw material is also more rational, makes producing ethylene from dehydration of ethanol technology attention.
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 (US4134926) 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, will cause the generation of other by products, but if increase flow velocity, the transformation efficiency of ethanol can decline again.In order to solve this contradiction, skill in the thermal insulation that United States Patent (USP) (US4232179) proposes ethanol dehydration reaction, namely ethanol dehydration reaction carries out in insulation fix bed, and 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 (US4396789), 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.Halcon/SD company develops the double mode technology of thermal insulation or isothermal fixed bed in nineteen seventies in addition, and 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 hours
-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 recovery of heat energy and the problem of organic wastewater treatment process in shorter mention producing ethylene from dehydration of ethanol, particularly reduce feed ethanol consumption and the energy-conservation technical problem of device.The organic waste water of current full scale plant is without the waste disposal plant outside the direct access to plant of process, one side is that organism, the particularly ethanol in organic waste water does not get utilization, ethanol consumption is increased, because organic concentration is higher in waste water on the other hand, the difficulty that waste disposal plant outside battery limit (BL) is disposed of sewage increases, and processing cost also increases.Patent CN101376551B proposes the organic waste water in the disposal methods producing ethylene from dehydration of ethanol of employing four cell process, there is complex process, long flow path, problem that investment is large.
Summary of the invention
Technical problem to be solved by this invention is that in prior art, producing ethylene from dehydration of ethanol energy recovery organic waste water that is insufficient and that produce fully is not processed, to reach the object of recycling, though or treated, there is complex process, long flow path, problem that investment is large, a kind of energy-saving production method of new producing ethylene from dehydration of ethanol is provided.The method has that technique is simple, less investment and energy-conservation feature.
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 energy-saving production method of producing ethylene from dehydration of ethanol, comprises the following steps:
A) by vapour phase ethanol and γ-Al
2o
3, ZSM molecular sieve, at least one catalyst exposure in molecular sieve or mordenite, there is dehydration reaction and generate logistics 2 containing ethene;
B) logistics 2 reclaims heat through heat reclaim unit, obtains the logistics (3) that temperature is down to 110 ~ 350 DEG C), heat reclaim unit reclaims heat and produces steam stream 8; ;
C) logistics 3 enters the bottom of quench tower, carries out cooling wash with the washing water counter current contact entered from quench tower top, and the top of quench tower obtains vapour phase crude ethylene logistics 5, and the bottom of quench tower obtains the liquid phase organic waste water logistics 6 containing ethanol, ether, ethene;
D) stripping rectifying is carried out in the middle and upper part that logistics 6 enters stripping rectifying tower, and tower top obtains the logistics 9 containing ethanol, ether, ethene, and tower reactor obtains aqueous stream 7, organic content≤20ppm in logistics 7;
E) logistics 8 is as thermal source, partly or entirely for the heating of stripping tower bottom of rectifying tower.
In technique scheme, preferably, ethanol dehydration reaction produces the reactor of ethene is calandria type fixed bed, multistage insulation fixed bed or single stage adiabatic fixed bed.
In technique scheme, preferably, the temperature of reaction of ethanol dehydration is 300 ~ 510 DEG C, and reaction pressure counts 0.01 ~ 5.0MPaG with gauge pressure, and reaction weight space velocity is 0.1 ~ 10 hour
-1.
In technique scheme, preferably, described quench tower is packing tower, tray column or void tower.
In technique scheme, preferably, the service temperature of quench tower is 30 ~ 120 DEG C, and working pressure counts 0.01 ~ 4.5MPaG with gauge pressure, and liquid gas weight ratio is 1.2 ~ 30, and theoretical plate number is 2 ~ 18.
In technique scheme, preferably, the service temperature of stripping rectifying tower is 30 ~ 210. 0 DEG C, and working pressure is 0 ~ 1.0MPaG, and theoretical plate number is 2 ~ 98, and the feed entrance point of organic waste water is at 1 ~ 85 theoretical tray place.
In technique scheme, preferably, described heat reclaim unit is waste heat boiler.
In technique scheme, preferably, the logistics 9 of stripping rectifying tower tower top is vapour phase or liquid phase extraction.
In technique scheme, preferably, when logistics 9 is vapour phase extraction, organic waste water logistics 6 feed entrance point is at column plate place, first piece, the top of stripping rectifying tower.
In technique scheme, preferably, when logistics 9 is liquid phase extraction, the reflux ratio of stripping rectifying tower is 0.1 ~ 6.
In the inventive method, the heat that heat reclaim unit reclaims is used for the heating of stripping tower bottom of rectifying tower.If this part heat is inadequate, also can passes into steam and do the bottom that thermal source directly enters tower at the bottom of stripping rectifying tower, also can with steam, deep fat, electricity etc. with the form of reboiler or well heater for stripping rectifying tower provides thermal source.
Reactant gases heat owing to being reclaimed by heat reclaim unit in the present invention is used as the thermal source of stripping rectifying tower, and adopt the organic waste water produced in stripping rectifying tower art breading producing ethylene from dehydration of ethanol, remove the organism of the ethanol in organic waste water, ether, ethene, carbon three and above hydrocarbon thereof, plant energy consumption decreases, organism in organic waste water, particularly ethanol get utilization, and reduce the consumption of feed ethanol.Adopt the inventive method, have that technique is simple, flow process is short, energy consumption is low and the feature of less investment, for the device of ton, coarse ethanol 222 tons/year (concentration is about 80 % by weight) in recyclable organic waste water, in organic waste water, organic concentration is down to trace from 0.265 % by weight, reclaims heat energy 44.776kw, amounts to and reduces steam 605 tons/year, reduce quench tower recirculated cooling water 234679 tons/year, achieve good 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 reactant gasess generated for dehydration reaction, 3 for reclaiming the reactant gases after heat, and 4 is the washing water of quench tower, and 5 is the crude ethylene gas after chilling washing, 6 is the organic waste water after chilling washing, and 7 is treated poor organic waste water, 8 steam occurred for waste heat boiler, 9 is the tower top material of stripping rectifying tower, 10 is oiler feed, and 1a is reactor, and 2a is waste heat boiler, 3a is quench tower, and 4a is stripping rectifying tower.
In Fig. 1, raw material vapour phase ethanol enters gas-solid and fixes bed bioreactor 1a, and containing γ-Al
2o
3, ZSM molecular sieve, molecular sieve or mordenite one or more catalyst exposure, dehydration reaction produces ethene and other by-product stream 2.Reactant gases 2 reclaims after heat through waste heat boiler 2a, enter gas chilled tower 3a, with washing water 4 chilling washing reaction gas, obtaining crude ethylene 5 after chilling washing goes follow up device to process, organic waste water 6 after chilling washing enters stripping rectifying tower 4a, isolate the logistics 9 containing ethanol, ether and ethene, carbon three and above hydrocarbon thereof at tower top, discharge aqueous stream 7 in tower reactor.Logistics 9 can be vapour phase extraction, also can be or liquid phase extraction.When logistics 9 is vapour phase extraction, organic waste water logistics 6 feed entrance point is at column plate place, first piece, stripping rectifying tower top.When logistics 9 is liquid phase extraction, reflux ratio is 0.1 ~ 6.
Below by embodiment, the present invention is further elaborated.
Embodiment
[embodiment 1]
By the technical scheme shown in Fig. 1, raw material vapour phase ethanol temperature of reaction 345 DEG C, reaction pressure 0.06MPaG, liquid phase ethanol air speed 0.9hr
-1condition under, with γ-Al
2o
3catalyst exposure dehydration reaction produces ethene, reactant gases reclaims after heat through waste heat boiler, temperature is down to 160 DEG C and is entered quench tower, wash with washing water under the condition of top pressure 0.04MPaG, top temperature 40 DEG C, liquid phase organic waste water after washing enters stripping rectifying tower and is separated, separate containing organic secondary organic wastewater at tower top, isolate the poor organic wastewater containing micro-content organism in tower reactor.The each composition flow rate of organic waste water is: carbonic acid gas 0.016 kg/hr, ethene 0.799 kg/hr, 0.002 kg/hr, ethane, 0.001 kg/hr, propane, 0.977 kg/hr, acetaldehyde, ethanol 22.229 kgs/hr, ether 0.398 kg/hr, heavy constituent 0.07 kg/hr, 9204.193 kgs/hr, water.The poor organic wastewater of stripping tower bottom of rectifying tower is 9200 kgs/hr, and wherein organism is 4ppm.Stripping rectifying tower overhead vapor phase enters condenser, flow is 103.596 kgs/hr, stripping rectifier column reflux 74.910 kgs/hr, and the extraction of stripping rectifying tower is rich in organic waste water 27.744 kgs/hr, alcohol concn 79.6%wt, stripping rectifying tower top gas phase 0.942 kg/hr.The tower top temperature of stripping rectifying tower is 90.8 DEG C, pressure is 0.11MPaG, bottom temperature is 125 DEG C, full tower theoretical plate number is 12, feed entrance point is at middle part, waste heat boiler reclaim heat all for stripping tower bottom of rectifying tower heating, in addition again with the form of reboiler for stripping rectifying tower provides thermal source.
Waste heat boiler reclaims heat energy 44.776kw, and the thermal load of stripping distillation tower reboiler is 578.635kw, annual saving low-pressure steam 605 tons; Reduce quench tower cooling load 35.7kw, amount to annual saving recirculated cooling water 234679 tons/year.
[embodiment 2]
Same embodiment [embodiment 1], the theoretical stage of a change stripping rectifying tower: full tower theoretical plate number is 22, and feed entrance point is in middle and upper part.The poor organic wastewater of stripping tower bottom of rectifying tower is 9200 kgs/hr, and wherein organism is 3ppm.Stripping rectifying tower overhead vapor phase enters condenser, flow is 40.577 kgs/hr, stripping rectifier column reflux 11.890 kgs/hr, and the extraction of stripping rectifying tower is rich in organic waste water 27.744 kgs/hr, alcohol concn 79.6%wt, stripping rectifying tower top gas phase 0.942 kg/hr.The tower top temperature of stripping rectifying tower is 90.8 DEG C, and pressure is 0.11MPaG, and bottom temperature is 125 DEG C.
Reactant gases temperature is down to 160 DEG C through waste heat boiler, reclaim heat all for stripping tower bottom of rectifying tower heating, in addition again with the form of reboiler for stripping rectifying tower provides thermal source.
Waste heat boiler reclaims heat energy 44.776kw, and the thermal load of stripping distillation tower reboiler is 557.833kw, annual saving low-pressure steam 605 tons; Reduce quench tower cooling load 35.7kw, amount to annual saving recirculated cooling water 234679 tons/year.
[embodiment 3]
With [embodiment 1], the tower reactor type of heating of a change stripping distillation tower, the bottom directly entering tower with steam replaces reboiler, and tower top frozen-free device, vapour phase extraction returns producing ethylene from dehydration of ethanol device.Organic waste water logistics 6 feed entrance point is at column plate place, first piece, the top of stripping rectifying tower.The poor organic wastewater of stripping tower bottom of rectifying tower is 10538.662 kgs/hr, and wherein organism is 12.7ppm.Stripping rectifying tower overhead vapor phase (being rich in organic waste water) flow is 240.024 kgs/hr, alcohol concn 9.23%wt.The tower top temperature of stripping rectifying tower is 120.5 DEG C, and pressure is 0.11MPaG, and bottom temperature is 123.3 DEG C.
Reactant gases temperature is down to 160 DEG C through waste heat boiler, reclaims heat all for the heating of stripping tower bottom of rectifying tower, and the form directly entered with steam more in addition provides thermal source for stripping rectifying tower.
Waste heat boiler reclaims heat energy 44.776kw, and the flow of stripping distillation tower stripped vapor is 11795 tons/year.Annual saving low-pressure steam 605 tons; Reduce quench tower cooling load 35.7kw, amount to annual saving recirculated cooling water 234679 tons/year.
Claims (10)
1. an energy-saving production method for producing ethylene from dehydration of ethanol, comprises the following steps:
A) by vapour phase ethanol and γ-Al
2o
3, ZSM molecular sieve, at least one catalyst exposure in molecular sieve or mordenite, there is dehydration reaction and generate logistics (2) containing ethene;
B) logistics (2) reclaims heat through heat reclaim unit, obtains the logistics (3) that temperature is down to 110 ~ 350 DEG C, and heat reclaim unit reclaims heat and produces steam stream (8);
C) logistics (3) enters the bottom of quench tower, carry out cooling with the washing water counter current contact entered from quench tower top to wash, the top of quench tower obtains vapour phase crude ethylene logistics (5), and the bottom of quench tower obtains the liquid phase organic waste water logistics (6) containing ethanol, ether, ethene;
D) stripping rectifying is carried out in the middle and upper part that logistics (6) enters stripping rectifying tower, tower top obtains the logistics (9) containing ethanol, ether, ethene, tower reactor obtains aqueous stream (7), organic content≤20ppm in logistics (7);
E) logistics (8) as thermal source, partly or entirely for the heating of stripping tower bottom of rectifying tower.
2. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that the reactor that ethanol dehydration reaction produces ethene is calandria type fixed bed, multistage insulation fixed bed or single stage adiabatic fixed bed.
3. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 1, it is characterized in that the temperature of reaction of ethanol dehydration is 300 ~ 510 DEG C, reaction pressure counts 0.01 ~ 5.0MPaG with gauge pressure, and reaction weight space velocity is 0.1 ~ 10 hour
-1.
4. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that described quench tower is packing tower, tray column or void tower.
5. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 1, it is characterized in that the service temperature of quench tower is 30 ~ 120 DEG C, working pressure counts 0.01 ~ 4.5MPaG with gauge pressure, and liquid gas weight ratio is 1.2 ~ 30, and theoretical plate number is 2 ~ 18.
6. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 1, it is characterized in that the service temperature of stripping rectifying tower is 30 ~ 210. 0 DEG C, working pressure is 0 ~ 1.0MPaG, and theoretical plate number is 2 ~ 98, and the feed entrance point of organic waste water is at 1 ~ 85 theoretical tray place.
7. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that described heat reclaim unit is waste heat boiler.
8. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 1, is characterized in that the logistics (9) of stripping rectifying tower tower top is vapour phase or liquid phase extraction.
9. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 8, is characterized in that, when logistics (9) is for vapour phase extraction, organic waste water logistics (6) feed entrance point is at column plate place, first piece, the top of stripping rectifying tower.
10. the energy-saving production method of producing ethylene from dehydration of ethanol according to claim 8, is characterized in that, when logistics (9) is for liquid phase extraction, the reflux ratio of stripping rectifying tower is 0.1 ~ 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106608787A (en) * | 2015-10-22 | 2017-05-03 | 中国石油化工股份有限公司 | Method for comprehensive utilization of heat in process of preparing ethene through ethanol dehydration |
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| 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 |
-
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)
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| 徐晓育等: "乙醇脱水制取乙烯的工业生产", 《日用化学工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106608787A (en) * | 2015-10-22 | 2017-05-03 | 中国石油化工股份有限公司 | Method for comprehensive utilization of heat in process of preparing ethene through ethanol dehydration |
| CN106608787B (en) * | 2015-10-22 | 2019-04-12 | 中国石油化工股份有限公司 | The method that heat integration utilizes in producing ethylene from dehydration of ethanol technique |
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