CN104610019B - The method producing dehydrated alcohol - Google Patents
The method producing dehydrated alcohol Download PDFInfo
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- CN104610019B CN104610019B CN201510061321.7A CN201510061321A CN104610019B CN 104610019 B CN104610019 B CN 104610019B CN 201510061321 A CN201510061321 A CN 201510061321A CN 104610019 B CN104610019 B CN 104610019B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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Abstract
The present invention relates to a kind of method producing dehydrated alcohol, mainly solve the problem that in prior art, energy consumption is high.The present invention is by using a kind of method producing dehydrated alcohol, comprise the steps: that (a) alcohol fermentation liquid is divided at least two parts, it is partly into rectifying column I, the ethanol stream I that concentration is 40～60wt% is obtained at rectifying column I top, it is partly into rectifying column II, obtains the ethanol stream II that concentration is 40～60wt% at rectifying column II top；B infiltration evaporation separator is sent in () described ethanol stream I and ethanol stream II mixing, obtain, after infiltration evaporation separator is dehydrated, the ethanol stream III that concentration is 85～95wt%；C () described ethanol stream III enters molecular sieve pressure swing adsorber, obtain the technical scheme that concentration is dehydrated alcohol product more than 99wt% and preferably solve the problems referred to above, can be used for during dehydrated alcohol produces.
Description
Technical field
The present invention relates to a kind of method producing dehydrated alcohol.
Background technology
Ethanol has a wide range of applications field in Organic Chemicals and organic solvent, is also the new bio of a kind of great potential
Fuel.In recent years, along with the in short supply of petroleum resources and it is non-renewable, the continuous of low-carbon economy is advocated simultaneously, raw
Thing fermentative Production biomass fuel ethanol causes to be paid close attention to widely.In the fermentation liquid that fermentation technology produces, in addition to ethanol,
Possibly together with substantial amounts of moisture and other a small amount of impurity.Therefore, fermentation liquid has to pass through refined to remove water therein and impurity,
To obtain the highly purified dehydrated alcohol that can be used as fuel additive.
Owing to there is substantial amounts of water in fermentation liquid, the technique that biomass fuel ethanol refines focuses primarily upon the dehydration work of ethanol
Skill.In traditional fuel ethanol production technique, mostly first pass through the low-concentration ethanol that the mode of distillation is come in concentrated broth,
Obtaining dehydrated alcohol by modes such as vacuum distillation method constant boiling rectification methods again, the common ground of these technology is to be required for be drained off
Material system completely vaporize, its process needs to consume huge latent heat of phase change, produces high energy consumption.
Traditional ethanol rectification process as described in patent CN 101157890A, a kind of fuel ethanol production equipment and method, be
The topping still of two-tower process and rectifying column are split as two topping stills and two rectifying columns respectively, form by wine with dregs tower, rectifying column,
Recovery tower three tower process produces alcohol fuel.Although in this flow process, only recovery tower one tower uses live steam heating, but reclaims
The thick capacity for liquor that tower processes is too big, and the live steam amount causing recovery tower to use is excessive；Additionally, the nothing after adsorption tower is dehydrated
The heat of water-ethanol steam is not obtained by, so the not up to optimization of whole system, energy consumption is the highest.
Relatively advanced has patent CN 102126921B, the patent provides three tower heating means of a kind of azeotropic ethanol processed:
Topping still, low-pressure distillation tower, high-pressure rectification tower three tower process is used to produce alcohol fuel.The live steam conduct that pressure is higher
One effect steam heats to high-pressure rectification tower, and high-pressure rectification column overhead gas heats to low-pressure distillation tower, and topping still heat is by molecular sieve
The dehydrated alcohol gas of dewatering unit and low-pressure distillation tower tower overhead gas provide.Only additional heat on essence tower in technique, relative to it
Front patent has improved, but still has the space reducing energy consumption.
The dehydration utilizing infiltrating and vaporizing membrane to carry out ethanol solution is a kind of novel isolation technics, and its principle is that water permeable membrane is to feed liquid
In hydrone selective pass through, in the opposite side of film, the vapor partial pressure of water is less than its saturated pressure, relies on this at film two
The difference of the steam partial pressure of side, makes hydrone constantly be penetrated through film, and is making side be vaporized into steam, thus be
The ethanol solution higher through surveying available concentration.The method, without consuming steam, has higher compared to traditional rectificating method
Capacity usage ratio, energy-saving effect is notable.
Summary of the invention
The technical problem to be solved is the problem that in prior art, energy consumption is high, it is provided that a kind of new production dehydrated alcohol
Method.The method, in dehydrated alcohol produces, has the advantage that energy consumption is low.
For solving the problems referred to above, the technical solution used in the present invention is as follows: a kind of method producing dehydrated alcohol, including as follows
Step: (a) alcohol fermentation liquid is divided at least two parts, is partly into rectifying column I, obtains dense at rectifying column I top
Degree is the ethanol stream I of 40～60wt%, is partly into rectifying column II, obtain at rectifying column II top concentration be 40～
The ethanol stream II of 60wt%；B infiltration evaporation separator, warp are sent in () described ethanol stream I and ethanol stream II mixing
Obtain, after the dehydration of infiltration evaporation separator, the ethanol stream III that concentration is 85～95wt%；C () described ethanol stream III enters
Molecular sieve pressure swing adsorber, obtaining concentration is the dehydrated alcohol product more than 99wt%.
In technique scheme, it is preferable that in described alcohol fermentation liquid, concentration of alcohol is 3～10% by weight, and ethanol is sent out
Ferment liquid enters the ratio by mass of rectifying column I and rectifying column II and is calculated as 0.6～1.5:1.
In technique scheme, it is highly preferred that concentration of alcohol is 5～8% by weight in described alcohol fermentation liquid.
In technique scheme, it is preferable that the number of plates of described rectifying column I is 20～30, tower top temperature is 60～80 DEG C,
Bottom temperature is 80～100 DEG C, and operation pressure is 30～70kPa, and feedboard position numerical digit from top to bottom is in the 2nd～6 piece of tower
At plate；The number of plates of rectifying column II is 20～28, and tower top temperature is 90～110 DEG C, and bottom temperature is 100～120 DEG C, behaviour
Being 130～170kPa as pressure, feedboard position numerical digit from top to bottom is at the 2nd～6 block of column plate.
In technique scheme, it is highly preferred that the number of plates of described rectifying column I is 23～27, tower top temperature is 65～78 DEG C,
Bottom temperature is 85～98 DEG C；The number of plates of rectifying column II is 23～27, and tower top temperature is 95～108 DEG C, and bottom temperature is
105～118 DEG C.
In technique scheme, it is preferable that described infiltration evaporation separator operating temperature is 60～80 DEG C, operation pressure be 20～
80kPa。
In technique scheme, it is preferable that the membrane material that described infiltration evaporation separator uses is selectivity water permeable membrane, is selected from
Organic membrane, inoranic membrane or organic-inorganic hybrid films, ethanol and wet concentration can be selected and pass through by described membrane material.
In technique scheme, it is highly preferred that described membrane material selected from silicoaluminophosphate molecular sieve membrane, chitosan film, polyvinyl alcohol film,
Polyetherimde films or polyvinyl alcohol-Na molecular screen membrane.
In technique scheme, it is preferable that the operation temperature of described molecular sieve pressure swing adsorber is 125～145 DEG C, operation pressure
Power is 220～280kPa.
The present invention uses above-mentioned preliminary rectification and infiltration vaporization coupling technique, sloughs the moisture in wood-based composites fermentation liquid.
Substitute the distillation operation in high concentration of alcohol stage innovatively with infiltration evaporation, infiltration evaporation device is divided into liquid-phase chamber and vapour phase
Room, aqueous fermentation liquid enters liquid-phase chamber, and film passes through the hydrone in feed liquid is selective, the steam of water in the opposite side of film
Dividing potential drop is less than its saturated pressure, relies on the difference of this steam partial pressure in film both sides, makes hydrone constantly be permeated logical
Cross film, thus opposite side obtains the ethanol solution that concentration is higher.This process does not consume steam, therefore greatly drops compared with rectification
Low energy consumption, has good economic benefit, achieves preferable technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the invention.
Fig. 2 is the general flow chart of document CN 102126920B.
In Fig. 1, A is rectifying column I, and B is rectifying column II, and C is infiltration evaporation separator, and D is molecular sieve pressure-variable adsorption
Device, 1 is alcohol fermentation liquid, and 2 is ethanol stream I and ethanol stream II mixed liquor, and 3 is infiltration evaporation separator discharging thing
Stream, 4 is molecular sieve pressure swing adsorber output streams.
In Fig. 2, E is topping still, and F is low-pressure distillation tower, and G is high-pressure rectification tower, and 11 is alcohol fermentation liquid, and 12 is thick
Wine logistics, 13 is azeotropic ethanol, and 14 is low-pressure distillation tower tower reactor logistics, and 15 is high-pressure rectification column overhead stream.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Detailed description of the invention
[embodiment 1]
Ethanol content be 5wt% fermentation liquor preheater heating after be divided into first, second part, first, second part
Weight ratio is 0.82:1, and Part I enters the top of rectifying column I, and after rectification, tower top obtains the ethanol thing of 45wt%
Stream I, the preheated device heat exchange of this ethanol stream I condenses；Part II material liquid enters the top of rectifying column II, after rectification,
Tower top obtains the ethanol stream II of 45wt%, and this ethanol stream II enters rectifying column I tower reactor the second reboiler heat exchange condensation, essence
Evaporate tower II tower reactor reboiler to be heated by live steam.Condensed ethanol stream I and ethanol stream II mix laggard to enter to permeate vapour
Separator, obtains the ethanol stream III of 90wt% after infiltration evaporation separator is dehydrated, and ethanol stream III is through saturated vapor mistake
Entering molecular sieve pressure swing adsorber after heat, it is cold that molecular sieve pressure swing adsorber overhead stream enters rectifying column I tower reactor the first reboiler
The dehydrated alcohol product of 99.5wt% is obtained after Ning.
Rectifying column I number of plates is 25, and feed entrance point is that at several 2nd block of column plate, operation pressure is 35kPa, tower
Top temperature is 68 DEG C, and bottom temperature is 85 DEG C.Rectifying column II number of plates is 26, and feed entrance point is the 2nd piece of tower from top to bottom
At plate, operation pressure is 135kPa, and tower top temperature is 103 DEG C, and bottom temperature is 114 DEG C.Infiltration evaporation separator operation
Temperature is 70 DEG C, and operation pressure is 60kPa.The membrane material that infiltration evaporation separator uses is polyvinyl alcohol film.Molecular sieve becomes
The operation temperature of pressure adsorber is 135 DEG C, and operation pressure is 250kPa.
Energy consumption is accounted result and is shown: steam consumption is 1.66 tons of steam/ton dehydrated alcohol product.
[embodiment 2]
According to the condition described in embodiment 1 and step, ethanol content be 3wt% fermentation liquor preheating after be divided into first, the
Two parts, the weight ratio of first, second part is 1.2:1, and the concentration of alcohol of ethanol stream I and ethanol stream II is
40wt%.
Rectifying column I number of plates is 28, and feed entrance point is that at several 5th block of column plate, operation pressure is 31kPa, tower
Top temperature is 67 DEG C, and bottom temperature is 82 DEG C.Rectifying column II number of plates is 28, and feed entrance point is the 5th piece of tower from top to bottom
At plate, operation pressure is 149kPa, and tower top temperature is 105 DEG C, and bottom temperature is 116 DEG C.Infiltration evaporation separator operation
Temperature is 65 DEG C, and operation pressure is 70kPa.The membrane material that infiltration evaporation separator uses is polyvinyl alcohol film.Molecular sieve becomes
The operation temperature of pressure adsorber is 140 DEG C, and operation pressure is 270kPa.
Energy consumption is accounted result and is shown: steam consumption is 2.31 tons of steam/ton dehydrated alcohol product.
[embodiment 3]
According to the condition described in embodiment 1 and step, ethanol content be 8wt% fermentation liquor preheating after be divided into first, the
Two parts, the weight ratio of first, second part is 0.72:1, and the concentration of alcohol of ethanol stream I and ethanol stream II is
50wt%.
Rectifying column I number of plates is 23, and feed entrance point is that at several 2nd block of column plate, operation pressure is 58kPa, tower
Top temperature is 74 DEG C, and bottom temperature is 89 DEG C.Rectifying column II number of plates is 24, and feed entrance point is the 2nd piece of tower from top to bottom
At plate, operation pressure is 158kPa, and tower top temperature is 108 DEG C, and bottom temperature is 118 DEG C.Infiltration evaporation separator operation
Temperature is 75 DEG C, and operation pressure is 50kPa.The membrane material that infiltration evaporation separator uses is polyvinyl alcohol film.Molecular sieve becomes
The operation temperature of pressure adsorber is 128 DEG C, and operation pressure is 230kPa.
Energy consumption is accounted result and is shown: steam consumption is 1.29 tons of steam/ton dehydrated alcohol product.
[comparative example]
Flow process as shown in Figure 2, ethanol content is the top of the fermentation liquid entrance topping still of 8wt%, after slightly evaporating, tower top
Obtaining the thick wine that ethanol content is 48wt%, tower reactor obtains the ethanol content useless mash less than 0.005wt%.Thick wine enters low
Pressure rectifying column bottom, after rectification, tower top obtains azeotropic ethanol fume, and azeotropic ethanol fume enters Molecular sieve dehydration units；
Tower reactor obtains the tower bottoms that ethanol content is 40wt%, enters the bottom of high-pressure rectification tower, and after rectification, tower reactor obtains waste water,
The condensed rear portion of logistics that tower top obtains enters low-pressure distillation tower top, and a part is back to high-pressure rectification tower top.
The topping still number of plates is 26, and feed entrance point is that from top to bottom at the 2nd block of column plate, operation pressure is 40kPa, tower top temperature
Degree is 60 DEG C, and bottom temperature is 81 DEG C.The low-pressure distillation tower number of plates is 50, and feed entrance point is the 48th block of column plate from top to bottom
Place, operation pressure is 130kPa, and tower top temperature is 85 DEG C, and bottom temperature is 92 DEG C.The high-pressure rectification tower number of plates is 68,
Feed entrance point is that from top to bottom at the 60th block of column plate, operation pressure is 500kPa, and tower top temperature is 125 DEG C, bottom temperature
It it is 153 DEG C.
Energy consumption is accounted result and is shown: steam consumption is 2.1 tons of steam/ton dehydrated alcohol product.
Claims (8)
1. the method producing dehydrated alcohol, comprises the steps:
A () alcohol fermentation liquid is divided at least two parts, be partly into rectifying column I, obtains at rectifying column I top
Concentration is the ethanol stream I of 40～60wt%, is partly into rectifying column II, obtains dense at rectifying column II top
Degree is the ethanol stream II of 40～60wt%；
B () described ethanol stream I and ethanol stream II are respectively through preheater, rectifying column I tower reactor the second reboiler
Infiltration evaporation separator is sent in rear mixing, and obtaining concentration after infiltration evaporation separator is dehydrated is 85～95wt%
Ethanol stream III；
C () described ethanol stream III is through saturated vapor overheated entrance molecular sieve pressure swing adsorber, molecular sieve pressure-variable adsorption
It is anhydrous more than 99wt% that device overhead stream obtains concentration after entering the condensation of rectifying column I tower reactor the first reboiler
Alcohol product；
Wherein, the number of plates of described rectifying column I is 20～30, and tower top temperature is 60～80 DEG C, bottom temperature
Being 80～100 DEG C, operation pressure is 30～70kPa, and feedboard position numerical digit from top to bottom is in the 2nd～6 piece of tower
At plate；The number of plates of rectifying column II is 20～28, and tower top temperature is 90～110 DEG C, bottom temperature be 100～
120 DEG C, operation pressure is 130～170kPa, and feedboard position numerical digit from top to bottom is at the 2nd～6 block of column plate.
The method producing dehydrated alcohol the most according to claim 1, it is characterised in that second in described alcohol fermentation liquid
Determining alcohol is 3～10% by weight, and alcohol fermentation liquid enters rectifying column I and the ratio by mass of rectifying column II
It is calculated as 0.6～1.5:1.
The method producing dehydrated alcohol the most according to claim 2, it is characterised in that second in described alcohol fermentation liquid
Determining alcohol is 5～8% by weight.
The method producing dehydrated alcohol the most according to claim 1, it is characterised in that the column plate of described rectifying column I
Number is 23～27, and tower top temperature is 65～78 DEG C, and bottom temperature is 85～98 DEG C；The number of plates of rectifying column II
Being 23～27, tower top temperature is 95～108 DEG C, and bottom temperature is 105～118 DEG C.
The method producing dehydrated alcohol the most according to claim 1, it is characterised in that described infiltration evaporation separator
Operation temperature is 60～80 DEG C, and operation pressure is 20～80kPa.
The method producing dehydrated alcohol the most according to claim 1, it is characterised in that described infiltration evaporation separator
The membrane material used is selectivity water permeable membrane, selected from organic membrane, inoranic membrane or organic-inorganic hybrid films, described film
Ethanol and wet concentration can be selected and pass through by material.
The method producing dehydrated alcohol the most according to claim 6, it is characterised in that described membrane material is selected from sial
Molecular screen membrane, chitosan film, polyvinyl alcohol film, polyetherimde films or polyvinyl alcohol-Na molecular screen membrane.
The method producing dehydrated alcohol the most according to claim 1, it is characterised in that described molecular sieve pressure-variable adsorption
The operation temperature of device is 125～145 DEG C, and operation pressure is 220～280kPa.
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| CN104610019B true CN104610019B (en) | 2017-01-04 |
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| CN105418368B (en) * | 2015-12-31 | 2017-12-26 | 江苏九天高科技股份有限公司 | A kind of technique and device for producing high straight alcohol |
| WO2024004742A1 (en) * | 2022-06-28 | 2024-01-04 | 日東電工株式会社 | Membrane separation system and method for operating membrane separation device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070401A (en) * | 2011-01-27 | 2011-05-25 | 南京大学 | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution |
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| JP4487045B2 (en) * | 2004-08-04 | 2010-06-23 | 独立行政法人産業技術総合研究所 | Membrane separation and purification system for fermented ethanol |
| AR086134A1 (en) * | 2011-04-26 | 2013-11-20 | Celanese Int Corp | SEPARATION PROCESS OF REDUCED ENERGY ALCOHOL WITH WATER REMOVAL |
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| CN102070401A (en) * | 2011-01-27 | 2011-05-25 | 南京大学 | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution |
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