CN110404285B - Four-tower distillation and membrane separation integrated system and method for distilling ethanol - Google Patents
Four-tower distillation and membrane separation integrated system and method for distilling ethanol Download PDFInfo
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- CN110404285B CN110404285B CN201910648880.6A CN201910648880A CN110404285B CN 110404285 B CN110404285 B CN 110404285B CN 201910648880 A CN201910648880 A CN 201910648880A CN 110404285 B CN110404285 B CN 110404285B
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 239000012528 membrane Substances 0.000 title claims abstract description 107
- 238000004821 distillation Methods 0.000 title claims abstract description 35
- 238000000926 separation method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002699 waste material Substances 0.000 claims abstract description 14
- 238000009833 condensation Methods 0.000 claims abstract description 9
- 230000005494 condensation Effects 0.000 claims abstract description 9
- 235000013405 beer Nutrition 0.000 claims description 44
- 238000003795 desorption Methods 0.000 claims description 31
- 238000007872 degassing Methods 0.000 claims description 25
- 239000000446 fuel Substances 0.000 claims description 14
- 239000002808 molecular sieve Substances 0.000 claims description 13
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 13
- 238000007670 refining Methods 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000000855 fermentation Methods 0.000 claims description 2
- 230000004151 fermentation Effects 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 238000005498 polishing Methods 0.000 abstract description 12
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 230000018044 dehydration Effects 0.000 description 10
- 238000006297 dehydration reaction Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 7
- 239000001760 fusel oil Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000012808 vapor phase Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000010865 sewage Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/001—Processes specially adapted for distillation or rectification of fermented solutions
- B01D3/003—Rectification of spirit
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/001—Processes specially adapted for distillation or rectification of fermented solutions
- B01D3/003—Rectification of spirit
- B01D3/004—Rectification of spirit by continuous methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/145—One step being separation by permeation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/225—Multiple stage diffusion
- B01D53/226—Multiple stage diffusion in serial connexion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
-
- 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
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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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
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
本发明公开了四塔蒸馏与膜分离集成系统，包括醪液预热器、负压醪塔、常压醪塔、中压精塔和高压精塔；高压精塔通过管路依次连接酒气过热器和膜分离装置；所述膜分离装置包括串联的低真空膜组件和高真空膜组件。上述的系统蒸馏乙醇的方法，包括以下步骤：A、发酵成熟醪脱去气体形成脱气醪；B、脱气醪中酒汽与废醪液分离；C、酒汽经冷凝后形成粗酒精，粗酒精经中压精塔蒸馏后进入高压精塔；D、进入高压精塔的酒精蒸汽，部分经过热后顺序进入低真空膜组件和高真空膜组件将乙醇和水分离。本发明避免了蒸馏过程中的跑酒现象，降低冷冻水和蒸汽的消耗量，节能环保。
The present invention discloses a four-tower distillation and membrane separation integrated system, including a mash preheater, a negative pressure mash tower, a normal pressure mash tower, a medium pressure polishing tower and a high pressure polishing tower; the high pressure polishing tower is sequentially connected to a wine vapor superheater and a membrane separation device through a pipeline; the membrane separation device includes a low vacuum membrane assembly and a high vacuum membrane assembly connected in series. The above-mentioned method for distilling ethanol in the system includes the following steps: A. removing gas from fermented mature mash to form degassed mash; B. separating wine vapor from waste mash in the degassed mash; C. forming crude alcohol after condensation of wine vapor, and entering the high pressure polishing tower after distillation in the medium pressure polishing tower; D. partially heating the alcohol vapor entering the high pressure polishing tower and sequentially entering the low vacuum membrane assembly and the high vacuum membrane assembly to separate ethanol and water. The present invention avoids the phenomenon of wine leakage during the distillation process, reduces the consumption of chilled water and steam, and is energy-saving and environmentally friendly.
Description
Technical Field
The invention relates to the technical field of ethanol production, in particular to a four-tower distillation and membrane separation integrated system and a method for distilling ethanol by using the same.
Background
Patent number 201810719237.3 discloses a system for producing fuel ethanol by double-coarse double-fine four-tower four-effect energy-saving distillation and a using method thereof, mainly comprising a negative pressure mash tower, a degassing section, a normal pressure mash tower, a medium pressure fine tower and a high pressure fine tower, wherein alcohol steam at the top of the medium pressure fine tower is extracted from fuel ethanol steam dehydrated by a molecular sieve and is used for heating the negative pressure mash tower.
Dehydration through molecular sieves has the following problems: ① The feeding and desorption processes of the molecular sieve are intermittently carried out, so that the pressure at the top of the combined tower is suddenly high and suddenly low, the vapor phase is fed into the molecular sieve for dehydration, the automatic control is not easy to realize, the distillation operation is unstable, and wine is easy to run out; ② The light wine produced in the molecular sieve dehydration process is large, the alcohol content in the light wine is about 25% of the finished product content, so that the light wine content required to be treated by the distillation system is increased, and the steam consumption is increased.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, it is an object of the present invention to provide a four-column distillation and membrane separation integrated system and a method for distilling ethanol thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
In a first aspect of the invention, a four column distillation and membrane separation integrated system is provided, comprising a mash preheater, a negative pressure mash column, a normal pressure mash column, a medium pressure polishing column and a high pressure polishing column; the high-pressure rectifying tower is sequentially connected with the wine gas superheater and the membrane separation device through pipelines; the membrane separation device comprises a low vacuum membrane component and a high vacuum membrane component which are connected in series; the inlet end of the low vacuum membrane component is connected with a wine gas superheater pipeline, and the outlet end of the low vacuum membrane component is connected with the inlet end of the high vacuum membrane component; the outlet end of the high vacuum membrane component is connected with a reboiler of the normal pressure mash tower; the outlet end of the low vacuum membrane component and the outlet end of the high vacuum membrane component are also respectively connected with an anhydrous vacuum pump through a desorption condenser I and a desorption condenser II.
Preferably, the low vacuum membrane module and the high vacuum membrane module each comprise a plurality of shell-and-tube membrane structures connected in series, each shell-and-tube membrane structure comprises a shell and an inner tube positioned in the shell, and the inner tube comprises a ceramic tube and a molecular sieve membrane covered on the outer surface of the ceramic tube.
The space between the outer shell and the inner tube is a shell side, the inner space of the inner tube is a tube side, negative pressure is pumped in the tube side, alcohol steam is introduced into the shell side, after the alcohol steam passes through the low vacuum membrane component and the high vacuum membrane component, the moisture in the finished product can reach below 0.5%, most of the moisture and a small amount of the ethanol penetrate through the inner tube, and the water and the small amount of the ethanol enter the desorption condenser through the tube side to be condensed and then enter the distillation section to be recovered.
The tube side outlet end of the low vacuum membrane component is connected with the desorption condenser I, and the tube side outlet end of the high vacuum membrane component is connected with the desorption condenser II. The shell side outlet end of the low vacuum membrane component is connected with the shell side inlet end of the high vacuum membrane component, and the shell side outlet end of the high vacuum membrane component is connected with the reboiler of the normal pressure mash tower.
Preferably, the atmospheric pressure beer column reboiler comprises an atmospheric pressure beer column reboiler I and an atmospheric pressure beer column reboiler II which respectively form a closed loop with the atmospheric pressure beer column through pipelines; the outlet end of the high vacuum membrane component is specifically connected with a reboiler II of the normal pressure mash tower.
Preferably, the mash preheater comprises a mash primary preheater, a mash secondary preheater and a mash tertiary preheater which are connected in series, and the normal pressure mash tower reboiler II is connected with the finished product cooler through the mash tertiary preheater by a pipeline.
Preferably, the outlet end of the desorption condenser I and the outlet end of the desorption condenser II are connected with the crude wine tank through pipelines.
In a second aspect of the present invention, there is provided a method for systematically distilling ethanol as described above, comprising the steps of:
A. degassing the fermented mash to form a degassed mash;
B. Separating the alcohol vapor from the waste mash in the deaerated mash;
C. Condensing the alcohol vapor to form crude alcohol, distilling the crude alcohol by a medium-pressure rectifying tower, and then entering a high-pressure rectifying tower;
D. Concentrating the alcohol vapor entering the high-pressure rectifying tower to alcohol vapor with alcohol content of more than 95% (v/v) at the tower top, sequentially entering a low-vacuum membrane component and a high-vacuum membrane component to separate ethanol from water after part of the alcohol vapor is heated, and entering an atmospheric pressure mash tower reboiler II to heat the atmospheric pressure mash tower; most of the water and a small amount of ethanol enter a desorption condenser I and a desorption condenser II for condensation and then enter a distillation section for recovery;
Wherein the vacuum degree of the low vacuum membrane component is 9-11kpa absolute pressure, and common circulating water is introduced into the desorption condenser I; the vacuum degree of the high vacuum membrane component is 2-4kpa absolute, and low-temperature chilled water at 1 ℃ is introduced into the desorption condenser II.
Preferably, in the step A, the fermented mature mash is preheated and then fed at the top of the degassing section of the negative pressure mash tower, part of mash after the gas-removed fermented mash enters the bottom of the degassing section flows into the negative pressure mash tower through a self-flow pipeline, and the rest of the fermented mash enters the top of the normal pressure mash tower after being preheated.
Preferably, in the step B, the deaerated mash is heated by the steam rising from the bottom of the tower while descending in the negative pressure mash tower and the normal pressure mash tower, the wine steam is separated from the waste mash, and the vinasse is discharged from the bottom of the tower and sent to a vinasse treatment system.
Preferably, in the step C, the alcohol vapors at the tops of the negative pressure beer column and the normal pressure beer column enter a crude alcohol tank after condensation, crude alcohol in the crude alcohol tank enters the lower part of the medium pressure rectifying column after being preheated, all the alcohol vapors at the top of the medium pressure rectifying column reflux after being condensed by a reboiler of the normal pressure beer column, and alcohol at the bottom of the medium pressure rectifying column enters the high pressure rectifying column after being preheated.
Preferably, in the step D, after partial alcohol is evaporated after entering a high-pressure refining tower, vapor-liquid mass transfer exchange is carried out on the partial alcohol and the reflux liquid at the tower top, the alcohol is gradually concentrated until the alcohol vapor part with the alcohol content of more than 95% (v/v) at the tower top passes through a hot and then film-removing separation device, and the alcohol and the water are separated through the device; all the rest parts are removed to an atmospheric pressure mash tower reboiler to heat an atmospheric pressure mash tower, and waste hot water at the tower bottom of the high-pressure rectifying tower is used for preheating crude alcohol and then is used for decontaminating the water treatment system;
condensing fuel ethanol steam, then entering a mash three-stage preheater to preheat fermented mash, and finally cooling by a finished product cooler to obtain a fuel ethanol finished product; the common circulating water is at 26-28 ℃.
The invention has the beneficial effects that:
(1) The wine steam enters the shell side of the membrane separation device, and the tube side is used for desorption, so that the separation and desorption processes are continuous and stable, the dehydration effect is good, the occupied area of equipment is small, the investment is small, and the energy conservation and the environmental protection are realized; the membrane dehydration is a continuous process, the working pressure is stable, no influence is caused on distillation, and the phenomenon of wine leakage is avoided.
(2) According to the principle, in order to reduce the consumption of chilled water, the condensation of the light alcohol vapor on the vacuum side of the membrane dehydration process is divided into two sections, the membrane separation device comprises a low-vacuum membrane component and a high-vacuum membrane component which are mutually connected in series, the light alcohol vapor in the low-vacuum membrane component is cooled by common circulating water, and the light alcohol vapor in the high-vacuum membrane component is cooled by low-temperature chilled water, so that compared with the traditional molecular sieve dehydration, the 2/3 of the consumption of chilled water is reduced by improving the structure.
(3) The traditional molecular sieve dehydration device has large light alcohol content, the alcohol content in the light alcohol accounts for about 25% of the finished product, the membrane separation device is used for simultaneously desorbing and separating, the light alcohol content in the light alcohol accounts for about 5 per mill of the finished product, the light alcohol content required to be treated in the distillation section is greatly reduced, and the steam consumption is reduced;
Meanwhile, the alcohol steam is extracted from the vapor phase of the high-pressure rectifying tower, the fuel alcohol steam dehydrated by the membrane is used for heating the normal-pressure mash tower, and compared with the traditional process that the alcohol steam is extracted from the vapor phase at the top of the medium-pressure rectifying tower and the fuel alcohol steam dehydrated by the molecular sieve is used for heating the negative-pressure mash tower, the alcohol steam is more utilized for one effect, so that the steam consumption is reduced, and the invention is more energy-saving;
The steam consumption of the whole process for producing one ton of fuel ethanol is not more than 1.0 ton, and compared with the traditional process, the steam consumption can be reduced by more than 30 percent.
(4) The four-tower distillation and the membrane separation device are not independent and are not simply combined, heat coupling exists between the four-tower distillation and the membrane separation device, the energy-saving effect cannot be achieved without combination of the four-tower distillation device and the membrane separation device, the purpose is particularly that ① extracts alcohol from the vapor phase of the high-pressure rectifying tower of the four-tower distillation section, and the alcohol vapor returns to the distillation section to heat the normal-pressure mash tower after being dehydrated by the membrane component, so that the heat recycling is realized; ② After the two are combined, the light wine amount is reduced to below 1% from the original 25%, and the load of alcohol recovery in the distillation section is reduced, so that the steam consumption is reduced; ③ After combination, the energy-saving effect is more obvious, and compared with the traditional three-tower three-effect distillation process and a molecular sieve dehydration device and the technology and the device for producing the fuel ethanol by double-coarse double-fine four-tower four-effect distillation, the steam is saved by more than 20 percent.
(5) By utilizing the advanced four-effect thermal coupling distillation process, only the high-pressure rectifying tower needs to generate steam to provide heat through a reboiler, the wine steam of the high-pressure rectifying tower provides heat for the medium-pressure rectifying tower through the reboiler, the wine steam of the medium-pressure rectifying tower and the finished absolute ethanol steam respectively provide heat for the normal-pressure mash tower through the reboiler, the wine steam of the normal-pressure mash tower provides heat for the negative-pressure mash tower through the reboiler, one-tower steam inlet is truly realized, the four-tower work is realized, the heat is fully utilized, and the steam consumption is reduced.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a schematic cross-sectional view of a shell-and-tube membrane structure of the present invention;
In the figure: 101. a primary mash preheater, 102, a secondary mash preheater, 103, a tertiary mash preheater, 2, a degassing section, 3, a degassing section condenser group, 4, a raw wine tank, 5, a distillation vacuum pump, 6, a negative pressure mash tower condenser group, 7, a finished product cooler, 8, a negative pressure mash tower, 9, a normal pressure mash tower feed preheater, 10, a normal pressure mash tower, 11, a negative pressure mash tower reboiler, 12, a vinasse treatment system, 13, a raw alcohol preheater, 14, a medium pressure rectifying tower, 15, a medium pressure rectifying tower reboiler, 16, a normal pressure mash tower reboiler I, 17, a high pressure rectifying tower feed preheater, 18, a high pressure rectifying tower, 19, a fusel oil separator, 20, a sewage treatment system, 21, a rectifying tower reboiler, 22, a condensate tank, 23, a boiler house, 24, a normal pressure mash tower reboiler II, 25, a wine gas superheater, 26, a low vacuum membrane module, 27, a high vacuum membrane module, 28, a desorption condenser I, 29, a desorption condenser II, 30, a non-water vacuum pump, 31, a housing, a ceramic membrane, 32, a ceramic membrane, 33, a molecular sieve, a tube side, and a tube side.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present application, the technical scheme of the present application will be described in detail with reference to specific embodiments.
The four-tower distillation and membrane separation integrated system comprises a mash preheater, a degassing section 2, a degassing section condenser set 3, a crude wine tank 4, a distillation vacuum pump 5, a negative pressure mash tower condenser set 6 and a finished product cooler 7. The mash preheater forms a closed loop with the degassing section 2 via a pipeline. In order to achieve better preheating effect and improve production efficiency, the mash preheater comprises a mash primary preheater 101, a mash secondary preheater 102 and a mash tertiary preheater 103 which are connected in series.
The outlet end of the mash third-stage preheater 103 is respectively connected with the finished product cooler 7 and the degassing section 2, the outlet end of the degassing section 2 is respectively connected with the raw wine tank 4 and the distillation vacuum pump 5 after passing through the mash first-stage preheater 101 and the degassing section condenser group 3 in sequence through a pipeline, and the outlet end of the negative pressure mash tower 8 is respectively connected with the raw wine tank 4 and the distillation vacuum pump 5 after passing through the mash second-stage preheater 102 and the negative pressure mash tower condenser group 6 in sequence through a pipeline.
The device also comprises a negative pressure beer column 8, a normal pressure beer column feeding preheater 9, a normal pressure beer column 10, a negative pressure beer column reboiler 11, a normal pressure beer column reboiler and a vinasse treatment system 12, wherein the outlet end of the degassing section 2 is connected with the negative pressure beer column 8 through a pipeline, the outlet end of the degassing section 2 is connected with the normal pressure beer column 10 after passing through the normal pressure beer column feeding preheater 9 through a pipeline, and the outlet end of the normal pressure beer column 10 is connected with the crude wine tank 4 after passing through the negative pressure beer column reboiler 11 through a pipeline.
The negative pressure beer column reboiler 11 forms a closed loop with the negative pressure beer column 8 through a pipeline, and the outlet end of the negative pressure beer column 8 is connected with the vinasse treatment system 12 through a pipeline.
The atmospheric pressure beer column reboiler comprises an atmospheric pressure beer column reboiler I16 and an atmospheric pressure beer column reboiler II 24 which respectively form a closed loop with the atmospheric pressure beer column 10 through pipelines; the normal pressure beer still 10 forms a closed loop with the normal pressure beer still reboiler I16 and the normal pressure beer still reboiler II 24 respectively through pipelines, and the outlet end of the normal pressure beer still 10 is connected with the vinasse treatment system 12 through pipelines after passing through the normal pressure beer still feeding preheater 9.
It also comprises a crude alcohol preheater 13, a medium pressure rectifying tower 14, a medium pressure rectifying tower reboiler 15, an atmospheric pressure mash tower reboiler I16, a high pressure rectifying tower feeding preheater 17, a high pressure rectifying tower 18, a fusel oil separator 19, a sewage treatment system 20, a rectifying tower reboiler 21, a condensate tank 22 and a boiler room 23.
The outlet end of the crude wine tank 4 is connected with a medium-pressure rectifying tower 14 through a pipeline after passing through a crude alcohol preheater 13, and the medium-pressure rectifying tower 14 forms a closed loop with a medium-pressure rectifying tower reboiler 15 and an atmospheric pressure mash tower reboiler I16 respectively through pipelines; the atmospheric beer column reboiler I16 is also in communication with the high pressure polishing column 18.
The outlet end of the medium pressure rectifying tower 14 is connected with the high pressure rectifying tower 18 through a pipeline after passing through the high pressure rectifying tower feeding preheater 17, and the high pressure rectifying tower 18 forms a closed loop with the medium pressure rectifying tower reboiler 15 and the rectifying tower reboiler 21 respectively through pipelines; the outlet end of the rectifying tower reboiler 21 is connected with a boiler room 23 after passing through a condensate tank 22 and a high-pressure rectifying tower feeding preheater 17 in sequence through a pipeline.
The outlet end of the high-pressure rectifying tower 18 is connected with a fusel oil separator 19 through a pipeline, and the outlet end of the high-pressure rectifying tower 18 is also connected with a sewage treatment system 20 through a pipeline and a crude alcohol preheater 13.
The high-pressure rectifying tower 18 is sequentially connected with a wine gas superheater 25 and a membrane separation device through pipelines; the membrane separation device comprises a low vacuum membrane module 26 and a high vacuum membrane module 27 which are connected in series; the inlet end of the low vacuum membrane component 26 is connected with the wine gas superheater 25 through a pipeline, and the outlet end of the low vacuum membrane component 26 is connected with the inlet end of the high vacuum membrane component 27; the outlet end of the high vacuum membrane component 27 is connected with an atmospheric pressure mash tower reboiler II 24; the outlet end of the low vacuum membrane module 26 and the outlet end of the high vacuum membrane module 27 are also connected with an anhydrous vacuum pump 30 through a desorption condenser I28 and a desorption condenser II 29 respectively. The reboiler II 24 of the normal pressure mash tower is connected with the finished product cooler 7 through a pipeline via the mash three-stage preheater 103. The outlet end of the desorption condenser I28 and the outlet end of the desorption condenser II 29 are connected with the crude wine tank 4 through pipelines.
The low vacuum membrane module 26 and the high vacuum membrane module 27 each comprise a plurality of shell-and-tube membrane structures connected in series, as shown in fig. 2, each shell-and-tube membrane structure comprises a shell 31 and an inner tube positioned inside the shell 31, wherein the inner tube comprises a ceramic tube 32 and a molecular sieve membrane 33 coated on the outer surface of the ceramic tube 32.
The space between the outer shell 31 and the inner tube is a shell side 34, the inner space of the inner tube is a tube side 35, negative pressure is pumped in the tube side 35, alcohol steam is introduced into the shell side 34, after the alcohol steam passes through the low vacuum membrane component 26 and the high vacuum membrane component 27, the moisture in the finished product can reach below 0.5%, most of the moisture and a small amount of ethanol penetrate through the inner tube, and the water and the small amount of ethanol enter a desorption condenser for condensation through the tube side 35 and then enter a distillation section for recovery.
The method for distilling ethanol by the system comprises the following steps:
A. The fermented mature mash is preheated by a mash preheater and then enters a degassing section 2, carbon dioxide and partial low boiling impurities in the mature mash are separated from the fermented mash under the action of negative pressure of the degassing section 2, the impurity-containing crude wine steam enters a mash primary preheater 101 and a degassing section condenser group 3 for condensation, and then condensate enters a crude wine tank 4; after the fermented mash with gas removed enters the bottom of the degassing section 2, part of mash (about 47%) flows into the negative pressure mash tower 8 through a self-flowing pipeline, and the rest (about 53%) enters the normal pressure mash tower 10 after being preheated by the normal pressure mash tower feeding preheater 9;
wherein: the deaerated mash is heated by the steam rising at the bottom of the negative pressure mash tower 8 while descending from the deaeration section 2 to the negative pressure mash tower 8, and the wine steam is separated from the waste mash; waste mash is discharged from the bottom of the negative pressure mash tower 8 and sent to the vinasse treatment system 12 for treatment; after the alcohol vapor of the negative pressure beer column 8 rises, part of the alcohol vapor enters the bottom of the degassing section 2, the rest crude alcohol vapor passes through the beer liquid preheater and then reaches the negative pressure beer column condenser group 6 to be condensed, and condensate enters the crude alcohol tank 4; the uncondensed impurity-containing gas is discharged through a distillation vacuum pump 5.
The mash preheater comprises a mash primary preheater 101, a mash secondary preheater 102 and a mash tertiary preheater 103 which are sequentially connected through pipelines, fermented mature mash is preheated to 45 ℃ by the mash primary preheater 101, the mash secondary preheater 102 is preheated to 55 ℃, the mash tertiary preheater 103 is preheated to about 61 ℃ and then enters a degassing section 2, carbon dioxide and part of low boiling impurities in the mature mash are separated from the fermented mash under the action of negative pressure of the degassing section 2, and the impurity-containing crude wine steam enters the mash primary preheater 101; the crude wine steam enters a mash secondary preheater 102 and a negative pressure mash tower condenser group 6 to be condensed, and the condensate enters a crude wine tank 4.
B. The partial deaerated mash entering the normal pressure mash tower 10 is heated by the rising steam at the bottom of the normal pressure mash tower 10 while descending in the normal pressure mash tower 10, and the rising of the wine steam is separated from the waste mash; the waste mash is discharged from the bottom of the normal pressure mash tower 10, and the waste mash is sent to the vinasse treatment system 12 for treatment after the fermented mash is preheated; the alcohol gas of the normal pressure beer still 10 goes upward to enter a negative pressure beer still reboiler 11 to heat the negative pressure beer still 8, and the condensed crude alcohol enters a crude alcohol tank 4; the tower top steam of the normal pressure beer column 10 heats the negative pressure beer column 8 through a negative pressure beer column reboiler 11. The operating temperature of the bottom of the negative pressure beer column 8 is 80 ℃, the top temperature is 65 ℃, and the top temperature of the degassing section 2 is 60 ℃.
C. the crude alcohol from the crude alcohol tank 4 enters the medium pressure rectifying tower 14 after being preheated by the crude alcohol preheater 13 (exchanging heat with waste hot water at the bottom of the high pressure rectifying tower 18), part of alcohol is evaporated after entering the tower and then exchanges gas-liquid mass transfer with the reflux liquid at the top of the tower, the alcohol vapor is gradually concentrated until the alcohol vapor with the alcohol content of 95% (v/v) or more at the top of the tower enters the constant pressure rectifying tower reboiler I16 to heat the constant pressure rectifying tower 10, part of alcohol vapor flows back after condensation, and the rest of alcohol vapor enters the top of the high pressure rectifying tower 18.
The medium pressure refining tower 14 is operated under positive pressure, the operating pressure is 0.25MPa, and the heating mode of the medium pressure refining tower 14 is as follows: the alcohol vapor at the top of the high-pressure rectifying tower 18 heats the medium-pressure rectifying tower 14 through the medium-pressure rectifying tower reboiler 15. The bottom operating temperature of the medium pressure rectifying tower 14 is 121 ℃ and the top temperature is 113 ℃.
D. The thin wine from the bottom of the medium pressure refining tower 14 enters the middle part of the high pressure refining tower 18 after being preheated by the feeding preheater 17 of the high pressure refining tower (exchanging heat with the steam condensate water), the alcohol is gradually concentrated after entering the tower until the alcohol concentration at the top of the tower can reach more than 95% (v/v), the medium-grade impurities (fusel oil) are retained on a plurality of layers of plates above the feeding plate, and the thin wine is extracted and cooled and enters the fusel oil separator 19 to separate the fusel oil. Alcohol vapor with alcohol content of more than 95% (v/v) is vapor phase extracted from the top of the high-pressure rectifying tower 18, enters a membrane separation device for dehydration through an alcohol gas superheater 25, and the rest alcohol vapor is totally refluxed after being condensed through a medium-pressure rectifying tower reboiler 15. And a decontaminating water treatment system 20 after the waste hot water of the tower bottom of the high-pressure rectifying tower 18 preheats the crude alcohol.
The high-pressure rectifying tower 18 works under positive pressure, the working pressure is 0.45MPa, and the heating mode of the high-pressure rectifying tower 18 is as follows: live steam from the boiler house heats the high pressure polishing column 18 through the high pressure polishing column 18 reboiler 21. The high pressure polishing column 18 had a column bottom operating temperature of 155℃and a top temperature of 126 ℃.
Alcohol vapor entering the membrane separation device firstly enters the low vacuum membrane component 26, the vacuum degree of the low vacuum membrane component 26 is 9-11kpa absolute, only ordinary circulating water (28 ℃) is needed to be condensed through the desorption condenser I28, and the low vacuum membrane component 26 can remove more than 65% of water in raw alcohol; alcohol vapor dehydrated by the low vacuum membrane assembly 26 enters the high vacuum membrane assembly 27, the vacuum degree of the high vacuum membrane assembly 27 is 2-4kpa absolute, low-temperature chilled water at 1 ℃ is required to be condensed by the desorption condenser II 29, and the high vacuum membrane assembly 27 can only remove 35% of water in raw alcohol. The device separates ethanol from water to finally obtain fuel ethanol. Condensing by a two-stage condenser, and saving the demand of chilled water.
The dehydrated fuel ethanol steam enters an atmospheric pressure mash tower reboiler II 24 to heat the atmospheric pressure mash tower 10, enters a mash three-stage preheater 103 to preheat fermentation mash after condensation, and finally is cooled by a finished product cooler 7 to obtain a fuel ethanol finished product.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (1)
1. The method for distilling ethanol by utilizing a four-tower distillation and membrane separation integrated system is characterized in that the four-tower distillation and membrane separation integrated system comprises a mash preheater, a negative pressure mash tower (8), an atmospheric mash tower (10), a medium pressure refining tower (14) and a high pressure refining tower (18); the method is characterized in that: the high-pressure rectifying tower (18) is sequentially connected with a wine gas superheater (25) and a membrane separation device through pipelines; the membrane separation device comprises a low vacuum membrane module (26) and a high vacuum membrane module (27) which are connected in series; the inlet end of the low vacuum membrane component (26) is connected with a pipeline of the wine gas superheater (25), and the outlet end of the low vacuum membrane component (26) is connected with the inlet end of the high vacuum membrane component (27); the outlet end of the high vacuum membrane component (27) is connected with a reboiler of the normal pressure mash tower; the outlet end of the low vacuum membrane component (26) and the outlet end of the high vacuum membrane component (27) are respectively connected with an anhydrous vacuum pump (30) through a desorption condenser I (28) and a desorption condenser II (29);
The low vacuum membrane assembly (26) and the high vacuum membrane assembly (27) comprise a plurality of shell-and-tube membrane structures connected in series, each shell-and-tube membrane structure comprises a shell (31) and an inner tube positioned inside the shell (31), and each inner tube comprises a ceramic tube (32) and a molecular sieve membrane (33) covered on the outer surface of the ceramic tube (32);
The constant pressure beer column reboiler comprises a constant pressure beer column reboiler I (16) and a constant pressure beer column reboiler II (24) which respectively form a closed loop with the constant pressure beer column (10) through pipelines; the outlet end of the high vacuum membrane component (27) is specifically connected with an atmospheric pressure mash tower reboiler II (24);
the mash preheater comprises a mash primary preheater (101), a mash secondary preheater (102) and a mash tertiary preheater (103), and the normal pressure mash tower reboiler II (24) is connected with the finished product cooler (7) through the mash tertiary preheater (103) by a pipeline;
The outlet end of the desorption condenser I (28) and the outlet end of the desorption condenser II (29) are connected with the crude wine tank (4) through pipelines;
The method comprises the following steps: A. degassing the fermented mash to form a degassed mash; B. separating the alcohol vapor from the waste mash in the deaerated mash; C. condensing the wine vapor to form crude alcohol, distilling the crude alcohol by a medium-pressure rectifying tower (14), and then entering a high-pressure rectifying tower (18); D. concentrating the alcohol vapor entering the high-pressure rectifying tower (18) to alcohol vapor with alcohol content of more than 95% (v/v) at the top of the tower, wherein a part of alcohol vapor enters the low-vacuum membrane component (26) and the high-vacuum membrane component (27) in sequence after being heated to separate ethanol from water, and the fuel alcohol vapor enters the normal-pressure mash tower reboiler II (24) to heat the normal-pressure mash tower (10); most of the water and a small amount of ethanol enter a desorption condenser I (28) and a desorption condenser II (29) for condensation and then enter a distillation section for recovery; wherein the vacuum degree of the low vacuum membrane component (26) is 9kpa to 11kpa absolute, and common circulating water is introduced into the desorption condenser I (28); the vacuum degree of the high vacuum membrane component (27) is 2kpa to 4kpa absolute, and the low temperature freezing at 1 ℃ is carried out in the desorption condenser II (29)
Water;
In the step A, the fermented mature mash is preheated and then is fed into the top of a degassing section (2) of a negative pressure mash tower (8), the fermented mash after gas removal enters the bottom of the degassing section (2), part of mash flows into the negative pressure mash tower (8) through a self-flowing pipeline, and the rest of fermented mash enters the top of an atmospheric pressure mash tower (10) after being preheated;
In the step B, the deaerated mash is heated by the rising steam at the bottom of the tower while descending in the negative pressure mash tower (8) and the normal pressure mash tower (10), the rising of the wine steam is separated from the waste mash, the vinasse is discharged at the bottom of the tower and sent to the vinasse treatment system (12);
In the step C, the alcohol gas at the tops of the negative pressure mash tower (8) and the normal pressure mash tower (10) enters a crude alcohol tank (4) after being condensed, the crude alcohol in the crude alcohol tank (4) enters the lower part of a medium pressure rectifying tower (14) after being preheated, the alcohol gas at the top of the medium pressure rectifying tower (14) completely flows back after being condensed by a reboiler of the normal pressure mash tower, and the alcohol at the bottom of the tower enters a high pressure rectifying tower (18) after being preheated;
In the step D, after the alcohol enters a high-pressure refining tower (18), part of the alcohol is evaporated and then carries out vapor-liquid mass transfer exchange with the reflux liquid at the top of the tower, the alcohol is gradually concentrated until the alcohol vapor part with the alcohol content of more than 95% (v/v) at the top of the tower passes through a hot and then film-removing separation device, and the alcohol and the water are separated through the device; all the rest parts are removed to an atmospheric pressure mash tower reboiler to heat an atmospheric pressure mash tower (10), and waste hot water at the tower bottom of a high-pressure rectifying tower (18) is used for preheating crude alcohol and then is used for decontaminating a water treatment system (20); the fuel ethanol vapor is condensed and then enters a mash three-stage preheater (103) to preheat fermentation mash, and finally is cooled by a finished product cooler (7) to obtain a fuel ethanol finished product; the common circulating water is at 26-28 ℃.
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| CN111072454B (en) * | 2020-01-19 | 2024-02-27 | 肥城金塔机械科技有限公司 | System and process for producing fuel ethanol by double-coarse and double-fine distillation with low pressure method |
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