CN104610019A - Method for producing absolute ethyl alcohol - Google Patents
Method for producing absolute ethyl alcohol Download PDFInfo
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- CN104610019A CN104610019A CN201510061321.7A CN201510061321A CN104610019A CN 104610019 A CN104610019 A CN 104610019A CN 201510061321 A CN201510061321 A CN 201510061321A CN 104610019 A CN104610019 A CN 104610019A
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- tower
- rectifying tower
- dehydrated alcohol
- ethanol
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention relates to a method for producing absolute ethyl alcohol, mainly aiming at solving the problem of high energy consumption in the prior art. The problems in the prior art are well solved by the technical scheme that the method for producing absolute ethyl alcohol comprises the following steps that (a) ethyl alcohol fermentation broth is divided into at least two parts, one part enters a rectifying tower I, an ethyl alcohol material flow I with the concentration of 40wt%-60wt% is obtained at the top of the rectifying tower I, the other part enters a rectifying tower II, and an ethyl alcohol material flow II with the concentration of 40wt%-60wt% is obtained at the top of the rectifying tower II; (b) the ethyl alcohol material flow I and the ethyl alcohol material flow II are mixed and sent into a pervaporation separator, and are dehydrated by the pervaporation separator to generate an ethyl alcohol material flow III with the concentration of 85wt%-95wt%; (c) the ethyl alcohol material flow III enters an element sieve absorption device to generate an absolute ethyl alcohol product with the concentration greater than 99wt%. The method can be applied to production of absolute ethyl alcohol.
Description
Technical field
The present invention relates to a kind of method of producing dehydrated alcohol.
Background technology
Ethanol has a wide range of applications field in Organic Chemicals and organic solvent, is also a kind of novel biological fuel of great potential.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, and biological fermentation process is produced biomass fuel ethanol and caused and pays close attention to widely.In the fermented liquid that zymotechnique is produced, except ethanol, also containing a large amount of moisture and other a small amount of impurity.Therefore, fermented liquid has to pass through refining to remove water wherein and impurity, to obtain the highly purified dehydrated alcohol that can be used as fuel dope.
Owing to there is a large amount of water in fermented liquid, the technique that biomass fuel ethanol is refined mainly concentrates on the dewatering process of ethanol.In traditional fuel ethanol production technique, the low-concentration ethanol in concentrated broth is mostly first carried out by the mode of distillation, dehydrated alcohol is obtained again by modes such as vacuum distillation method constant boiling rectification methods, the common ground of these technology all needs material system to be drained off to vaporize completely, its process need consumes huge latent heat of phase change, produces high energy consumption.
Traditional ethanol rectification process is as described in patent CN 101157890A, a kind of fuel ethanol production equipment and method, be that the topping still of two-tower process and rectifying tower are split as two topping stills and two rectifying tower respectively, form and produce alcohol fuel by wine with dregs tower, rectifying tower, recovery tower three tower process.Although only there is recovery tower one tower to use live steam heating in this flow process, the thick capacity for liquor of recovery tower process is too large, and the live steam amount causing recovery tower to use is excessive; In addition, the heat of dehydrated alcohol steam after adsorption tower dehydration is not utilized, so whole system do not reach optimization, energy consumption is very high.
Comparatively advanced has patent CN 102126921B, the patent provides a kind of three tower heating means of azeotropic ethanol processed: adopt topping still, low-pressure distillation tower, high-pressure rectification tower three tower process to produce alcohol fuel.The higher live steam of pressure is as an effect steam to the heating of high-pressure rectification tower, and high-pressure rectification column overhead gas heats to low-pressure distillation tower, and topping still heat is provided by the dehydrated alcohol gas of Molecular sieve dehydration units and low-pressure distillation tower overhead gas.Only external heat amount on smart tower in technique, relative to the progress to some extent of patent before, but still has the space reducing energy consumption.
The dehydration utilizing infiltrating and vaporizing membrane to carry out ethanolic soln is a kind of novel isolation technique, its principle be water permeable membrane to the water molecules in feed liquid selective through, in the opposite side of film, the vapor partial pressure of water is less than its saturated pressure, rely on the difference of this steam partial pressure in film both sides, water molecules is made constantly to be penetrated through film, and making side be vaporized into steam, thus for the higher ethanolic soln of concentration can be obtained through survey.The method is without the need to consuming steam, and have higher capacity usage ratio compared to traditional rectificating method, energy-saving effect is remarkable.
Summary of the invention
Technical problem to be solved by this invention is the problem that in prior art, energy consumption is high, provides a kind of method of production dehydrated alcohol newly.The method is used for, in dehydrated alcohol production, having the advantage that energy consumption is low.
For solving the problem, the technical solution used in the present invention is as follows: a kind of method of producing dehydrated alcohol, comprise the steps: that (a) ethanol fermentation liquid is divided at least two portions, a part enters rectifying tower I, the ethanol stream I that concentration is 40 ~ 60wt% is obtained at rectifying tower I top, a part enters rectifying tower II, obtains at rectifying tower II top the ethanol stream II that concentration is 40 ~ 60wt%; B () described ethanol stream I and ethanol stream II mix sends into infiltration evaporation separator, after the dehydration of infiltration evaporation separator, obtain 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 being greater than 99wt%.
In technique scheme, preferably, in described ethanol fermentation liquid, alcohol concn is 3 ~ 10% by weight, and the ratio by mass that ethanol fermentation liquid enters rectifying tower I and rectifying tower II counts 0.6 ~ 1.5:1.
In technique scheme, more preferably, in described ethanol fermentation liquid, alcohol concn is 5 ~ 8% by weight.
In technique scheme, preferably, the stage number of described rectifying tower I is 20 ~ 30, and tower top temperature is 60 ~ 80 DEG C, and bottom temperature is 80 ~ 100 DEG C, and working pressure is 30 ~ 70kPa, feed plate position from top to bottom numerical digit in 2nd ~ 6 pieces of column plate places; The stage number of rectifying tower II is 20 ~ 28, and tower top temperature is 90 ~ 110 DEG C, and bottom temperature is 100 ~ 120 DEG C, and working pressure is 130 ~ 170kPa, feed plate position from top to bottom numerical digit in 2nd ~ 6 pieces of column plate places.
In technique scheme, more preferably, the stage number of described rectifying tower I is 23 ~ 27, and tower top temperature is 65 ~ 78 DEG C, and bottom temperature is 85 ~ 98 DEG C; The stage number of rectifying tower II is 23 ~ 27, and tower top temperature is 95 ~ 108 DEG C, and bottom temperature is 105 ~ 118 DEG C.
In technique scheme, preferably, described infiltration evaporation separator operating temperature is 60 ~ 80 DEG C, and working pressure is 20 ~ 80kPa.
In technique scheme, preferably, the mould material that described infiltration evaporation separator uses is selectivity water permeable membrane, is selected from organic membrane, mineral membrane or organic-inorganic hybrid films, described mould material can to ethanol and wet concentration select through.
In technique scheme, more preferably, described mould material is selected from silicoaluminophosphate molecular sieve membrane, chitosan film, polyvinyl alcohol film, polyetherimde films or polyvinyl alcohol-Na molecular screen membrane.
In technique scheme, preferably, the service temperature of described molecular sieve pressure swing adsorber is 125 ~ 145 DEG C, and working pressure is 220 ~ 280kPa.
The present invention adopts above-mentioned preliminary rectifying and infiltration vaporization coupling technique, sloughs the moisture in wood-based composites fermented liquid.The distillation operation in high alcohol concn stage is substituted innovatively with infiltration evaporation, infiltration evaporation device is divided into liquid-phase chamber and vapour phase room, moisture fermented liquid enters liquid-phase chamber, film to the water molecules in feed liquid selective through, in the opposite side of film, the vapor partial pressure of water is less than its saturated pressure, rely on the difference of this steam partial pressure in film both sides, make water molecules constantly be penetrated through film, thus opposite side obtains the higher ethanolic soln of concentration.This process does not consume steam, therefore greatly reduces energy consumption compared with rectifying, has good economic benefit, achieves good 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 tower I, B is rectifying tower II, C is infiltration evaporation separator, and D is molecular sieve pressure swing adsorber, and 1 is ethanol fermentation liquid, 2 is ethanol stream I and ethanol stream II mixed solution, and 3 is infiltration evaporation separator output streams, and 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 ethanol fermentation liquid, and 12 is thick wine logistics, and 13 is azeotropic ethanol, and 14 is the logistics of low-pressure distillation tower tower reactor, and 15 is high-pressure rectification column overhead stream.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
Ethanol content is be divided into first, second part after the fermentation liquor preheater heating of 5wt%, the weight ratio of first, second part is 0.82:1, first part enters the top of rectifying tower I, after rectifying, tower top obtains the ethanol stream I of 45wt%, and this ethanol stream I is through preheater heat exchange condensation; Second section stock liquid enters the top of rectifying tower II, and after rectifying, tower top obtains the ethanol stream II of 45wt%, and this ethanol stream II enters rectifying tower I tower reactor second reboiler heat exchange condensation, and rectifying tower II tower reactor reboiler is heated by live steam.Condensed ethanol stream I and ethanol stream II mix laggardly to enter to permeate vaporization separator, the ethanol stream III of 90wt% is obtained after the dehydration of infiltration evaporation separator, ethanol stream III enters molecular sieve pressure swing adsorber after saturation steam is overheated, and molecular sieve pressure swing adsorber overhead stream obtains the dehydrated alcohol product of 99.5wt% after entering the condensation of rectifying tower I tower reactor first reboiler.
Rectifying tower I stage number is 25, and feed entrance point is several 2nd piece of column plate place from top to bottom, and working pressure is 35kPa, and tower top temperature is 68 DEG C, and bottom temperature is 85 DEG C.Rectifying tower II stage number is 26, and feed entrance point is the 2nd piece of column plate place from top to bottom, and working pressure is 135kPa, and tower top temperature is 103 DEG C, and bottom temperature is 114 DEG C.Infiltration evaporation separator operating temperature is 70 DEG C, and working pressure is 60kPa.The mould material that infiltration evaporation separator uses is polyvinyl alcohol film.The service temperature of molecular sieve pressure swing adsorber is 135 DEG C, and working 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 is be divided into first, second part after the fermentation liquor preheating of 3wt%, and the weight ratio of first, second part is 1.2:1, and the alcohol concn of ethanol stream I and ethanol stream II is 40wt%.
Rectifying tower I stage number is 28, and feed entrance point is several 5th piece of column plate place from top to bottom, and working pressure is 31kPa, and tower top temperature is 67 DEG C, and bottom temperature is 82 DEG C.Rectifying tower II stage number is 28, and feed entrance point is the 5th piece of column plate place from top to bottom, and working pressure is 149kPa, and tower top temperature is 105 DEG C, and bottom temperature is 116 DEG C.Infiltration evaporation separator operating temperature is 65 DEG C, and working pressure is 70kPa.The mould material that infiltration evaporation separator uses is polyvinyl alcohol film.The service temperature of molecular sieve pressure swing adsorber is 140 DEG C, and working 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 is be divided into first, second part after the fermentation liquor preheating of 8wt%, and the weight ratio of first, second part is 0.72:1, and the alcohol concn of ethanol stream I and ethanol stream II is 50wt%.
Rectifying tower I stage number is 23, and feed entrance point is several 2nd piece of column plate place from top to bottom, and working pressure is 58kPa, and tower top temperature is 74 DEG C, and bottom temperature is 89 DEG C.Rectifying tower II stage number is 24, and feed entrance point is the 2nd piece of column plate place from top to bottom, and working pressure is 158kPa, and tower top temperature is 108 DEG C, and bottom temperature is 118 DEG C.Infiltration evaporation separator operating temperature is 75 DEG C, and working pressure is 50kPa.The mould material that infiltration evaporation separator uses is polyvinyl alcohol film.The service temperature of molecular sieve pressure swing adsorber is 128 DEG C, and working 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 that the fermented liquid of 8wt% enters topping still, and after slightly heating up in a steamer, tower top obtains the thick wine that ethanol content is 48wt%, and tower reactor obtains the useless mash that ethanol content is less than 0.005wt%.Thick wine enters low-pressure distillation tower bottom, and after rectifying, 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 rectifying, tower reactor obtains waste water, and the logistics that tower top obtains enters low-pressure distillation tower top through condensation rear portion, and a part is back to high-pressure rectification tower top.
Topping still stage number is 26, and feed entrance point is the 2nd piece of column plate place from top to bottom, and working pressure is 40kPa, and tower top temperature is 60 DEG C, and bottom temperature is 81 DEG C.Low-pressure distillation tower stage number is 50, and feed entrance point is the 48th piece of column plate place from top to bottom, and working pressure is 130kPa, and tower top temperature is 85 DEG C, and bottom temperature is 92 DEG C.High-pressure rectification tower stage number is 68, and feed entrance point is the 60th piece of column plate place from top to bottom, and working pressure is 500kPa, and tower top temperature is 125 DEG C, and bottom temperature 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 (9)
1. produce a method for dehydrated alcohol, comprise the steps:
A () ethanol fermentation liquid is divided at least two portions, a part enters rectifying tower I, obtain at rectifying tower I top the ethanol stream I that concentration is 40 ~ 60wt%, a part enters rectifying tower II, obtains at rectifying tower II top the ethanol stream II that concentration is 40 ~ 60wt%;
B () described ethanol stream I and ethanol stream II mix sends into infiltration evaporation separator, after the dehydration of infiltration evaporation separator, obtain 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 being greater than 99wt%.
2. produce the method for dehydrated alcohol according to claim 1, it is characterized in that in described ethanol fermentation liquid, alcohol concn is 3 ~ 10% by weight, the ratio by mass that ethanol fermentation liquid enters rectifying tower I and rectifying tower II counts 0.6 ~ 1.5:1.
3. produce the method for dehydrated alcohol according to claim 2, it is characterized in that in described ethanol fermentation liquid, alcohol concn is 5 ~ 8% by weight.
4. produce the method for dehydrated alcohol according to claim 1, it is characterized in that the stage number of described rectifying tower I is 20 ~ 30, tower top temperature is 60 ~ 80 DEG C, and bottom temperature is 80 ~ 100 DEG C, working pressure is 30 ~ 70kPa, feed plate position from top to bottom numerical digit in 2nd ~ 6 pieces of column plate places; The stage number of rectifying tower II is 20 ~ 28, and tower top temperature is 90 ~ 110 DEG C, and bottom temperature is 100 ~ 120 DEG C, and working pressure is 130 ~ 170kPa, feed plate position from top to bottom numerical digit in 2nd ~ 6 pieces of column plate places.
5. produce the method for dehydrated alcohol according to claim 4, it is characterized in that the stage number of described rectifying tower I is 23 ~ 27, tower top temperature is 65 ~ 78 DEG C, and bottom temperature is 85 ~ 98 DEG C; The stage number of rectifying tower II is 23 ~ 27, and tower top temperature is 95 ~ 108 DEG C, and bottom temperature is 105 ~ 118 DEG C.
6. produce the method for dehydrated alcohol according to claim 1, it is characterized in that described infiltration evaporation separator operating temperature is 60 ~ 80 DEG C, working pressure is 20 ~ 80kPa.
7. produce the method for dehydrated alcohol according to claim 1, it is characterized in that the mould material that described infiltration evaporation separator uses is selectivity water permeable membrane, be selected from organic membrane, mineral membrane or organic-inorganic hybrid films, described mould material can to ethanol and wet concentration select through.
8. produce the method for dehydrated alcohol according to claim 7, it is characterized in that described mould material is selected from silicoaluminophosphate molecular sieve membrane, chitosan film, polyvinyl alcohol film, polyetherimde films or polyvinyl alcohol-Na molecular screen membrane.
9. produce the method for dehydrated alcohol according to claim 1, it is characterized in that the service temperature of described molecular sieve pressure swing adsorber is 125 ~ 145 DEG C, working pressure is 220 ~ 280kPa.
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| CN201510061321.7A CN104610019B (en) | 2015-02-05 | 2015-02-05 | The method producing dehydrated alcohol |
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| CN201510061321.7A CN104610019B (en) | 2015-02-05 | 2015-02-05 | The method producing dehydrated alcohol |
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| CN104610019B CN104610019B (en) | 2017-01-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418368A (en) * | 2015-12-31 | 2016-03-23 | 江苏九天高科技股份有限公司 | Technology and device for producing high-purity ethyl 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006042673A (en) * | 2004-08-04 | 2006-02-16 | National Institute Of Advanced Industrial & Technology | Membrane-separating/purifying system of fermented ethanol |
| CN102070401A (en) * | 2011-01-27 | 2011-05-25 | 南京大学 | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution |
| CN103108854A (en) * | 2011-04-26 | 2013-05-15 | 国际人造丝公司 | Reduced energy alcohol separation process having water removal |
-
2015
- 2015-02-05 CN CN201510061321.7A patent/CN104610019B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006042673A (en) * | 2004-08-04 | 2006-02-16 | National Institute Of Advanced Industrial & Technology | Membrane-separating/purifying system of fermented ethanol |
| CN102070401A (en) * | 2011-01-27 | 2011-05-25 | 南京大学 | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution |
| CN103108854A (en) * | 2011-04-26 | 2013-05-15 | 国际人造丝公司 | Reduced energy alcohol separation process having water removal |
Non-Patent Citations (1)
| Title |
|---|
| 陈林君: "节能的乙醇-水溶液分离技术", 《食品与发酵工业》, no. 2, 31 December 1992 (1992-12-31), pages 78 - 82 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418368A (en) * | 2015-12-31 | 2016-03-23 | 江苏九天高科技股份有限公司 | Technology and device for producing high-purity ethyl 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 |
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| CN104610019B (en) | 2017-01-04 |
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