CN102126923B - Three-tower differential pressure distillation method for preparing azeotropic ethanol - Google Patents

Three-tower differential pressure distillation method for preparing azeotropic ethanol Download PDF

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CN102126923B
CN102126923B CN 201010022747 CN201010022747A CN102126923B CN 102126923 B CN102126923 B CN 102126923B CN 201010022747 CN201010022747 CN 201010022747 CN 201010022747 A CN201010022747 A CN 201010022747A CN 102126923 B CN102126923 B CN 102126923B
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azeotropic ethanol
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CN102126923A (en
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韩飞
缪晡
石荣华
丁伟军
林长骏
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China Petrochemical Corp
Sinopec Shanghai Engineering Co Ltd
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Abstract

The invention relates to a three-tower differential pressure distillation method for preparing azeotropic ethanol, which mainly solves the problems of high energy consumption and high probability of material coking and tower plate blockage in towers in the prior art. The method comprises the following steps of: a) adding fermentation mash into the upper part of a coarse distillation tower I and performing coarse distillation to obtain a material flow 2 on the top of the tower and waste dregs in the kettle of the tower; b) adding the material flow 2 into the lower part of a rectification tower II and rectifying to obtain an azeotropic ethanol product on the top of the tower and a material flow 5 in the kettle of the tower; and c) adding the material flow 5 into the lower part of a rectification tower III and rectifying to obtain a material flow 8 on the top of the tower and rectification tower wastewater in the kettle of the tower, wherein the material flow 8 is divided into a material flow 6 and a material flow 7, the material flow 6 is added into the top of the rectification tower II and the material flow 7 flows back to the top of the rectification tower III. By the technical scheme, the problems are preferably solved; and the method can be applied in the industrial production process for preparing the azeotropic ethanol by three-tower differential pressure distillation.

Description

The three-tower differential pressure distillating method of azeotropic ethanol processed
Technical field
The present invention relates to a kind of three-tower differential pressure distillating method of azeotropic ethanol processed.
Background technology
The worsening shortages of petroleum resources, the demanding urgently of natural environment deterioration improve, and alcohol fuel is little as a kind of environmental pollution, and the energy of alternative oil receives the concern of various countries.Alcohol fuel is as a kind of alternative fuel of gasoline, the energy that burning is emitted is certain, and the energy consumption of producing alcohol fuel must be far smaller than the energy that burning is emitted, otherwise promoting the use of of alcohol fuel will be restricted, therefore, the production power saving of alcohol fuel is more and more outstanding.Yet the energy consumption of producing alcohol fuel mainly concentrates on distillation dehydration workshop section, and the energy consumption that reduces distillation dehydration workshop section is crucial.
Document CN101085717A provides a kind of processing method that adopts three-tower heat integration device to carry out ethanol distillation: adopt thick tower, low pressure azeotropy rectification column, high pressure azeotropy rectification column three tower process to produce alcohol fuel and edible ethanol.Enter the low pressure azeotropy rectification column from the topping still side line with the thick wine of gas phase form extraction in this flow process, enter high pressure azeotropy rectification column return tank by low pressure azeotropy rectification column top side line extraction part azeotropic alcohol, as the phegma of high pressure azeotropy rectification column, low pressure azeotropy rectification column tower reactor material enters the middle part of high pressure azeotropy rectification column together with the lime set of high pressure azeotropy rectification column top gaseous phase.The live steam that pressure is higher heats to high pressure azeotropy rectification column tower reactor, and the overhead gas of high pressure azeotropy rectification column is to the heating of topping still tower reactor, and live steam two effects are utilized.Although the document discloses the working pressure of thick tower in specification sheets be 10~300kPa, the working pressure of low pressure azeotropy rectification column is 10~280kPa, and the working pressure of high pressure azeotropy rectification column is 200~1200kPa.But in an embodiment, the working pressure of thick tower, low pressure azeotropy rectification column and high pressure azeotropy rectification column is respectively 140kPa, 110kPa and 580kPa.This shows, three towers, particularly thick tower are all operations under pressurization in the document, and thick tower working pressure is higher than the working pressure of low pressure azeotropy rectification column, the pressure of high pressure azeotropy rectification column is also higher, in three towers, temperature is corresponding higher, thereby the also corresponding rising of the pressure of needed water vapor, corresponding also corresponding increase of energy consumption.In addition, thick tower working pressure is high, and column plate is stopped up in easily coking in tower, is unfavorable for the long period steady running of device.
Summary of the invention
Technical problem to be solved by this invention is to have in prior art that energy consumption is high, the easy coking of material in tower, stop up the problem of column plate, and a kind of three-tower differential pressure distillating method of new azeotropic ethanol processed is provided.It is low that the method has energy consumption, and it is low that thick tower includes the wine with dregs portion temperature, the not susceptible to plugging characteristics of column plate.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of three-tower differential pressure distillating method of azeotropic ethanol processed comprises the following steps:
A) fermentation liquid enters the top of topping still I, and after slightly heating up in a steamer, tower top obtains logistics 2, and tower reactor obtains useless grain;
B) logistics 2 enters smart tower II bottom, and after rectifying, tower top obtains the product azeotropic ethanol, and tower reactor obtains logistics 5;
C) logistics 5 enters smart tower III bottom, and after rectifying, tower top obtains logistics 8, and tower reactor obtains smart tower waste water; Wherein, described logistics 8 is divided into logistics 6 and logistics 7 two portions, and logistics 6 enters smart tower II top, and logistics 7 is back to smart tower III top.
In technique scheme, the operational condition preferable range of topping still I is: the stage number preferable range is 20~30, and more preferably scope is 22~28; The tower top temperature preferable range is 50~70 ℃, and more preferably scope is 53~65 ℃; Tower reactor temperature preferable range is 70~100 ℃, and more preferably scope is 75~90 ℃; Working pressure P IPreferable range is 10kPa<P I<101.3kPa,, more preferably scope is 10kPa<P I<50kPa, perhaps 50kPa<P I<101.3kPa, most preferred range is 20kPa<P I<50kPa, perhaps 50kPa<P I<70kPa, particularly preferably scope is 30kPa<P I<50kPa, perhaps 50kPa<P I<60kPa; Feed plate location optimization scheme is for being positioned at from top to bottom the 2nd~10 column plate place.The operational condition preferable range of essence tower II is: the stage number preferable range is 40~70, and more preferably scope is 50~65; The tower top temperature preferable range is 75~100 ℃, and more preferably scope is 80~90 ℃; Tower reactor temperature preferable range is 80~110 ℃, and more preferably scope is 85~100 ℃; The working pressure preferable range is 50~500kPa, and more preferably scope is 60~400kPa, and most preferred range is 100~200kPa; The feed plate position is positioned at from top to bottom the 40th~50 column plate place.The operational condition preferable range of essence tower III is: the stage number preferable range is 50~80, and more preferably scope is 65~75; The tower top temperature preferable range is 100~140 ℃, and more preferably scope is 110~130 ℃; Tower reactor temperature preferable range is 120~160 ℃, and more preferably scope is 125~145 ℃; The working pressure preferable range is 100~800kPa, and more preferably scope is 200~700kPa, and most preferred range is 350~550kPa; The feed plate position is positioned at from top to bottom the 55th~65 column plate place.The working pressure preferred version of topping still I, smart tower II and smart tower III is that pressure increases successively.Logistics 6 is that preferable range is 1/4~1: 1 with the weight ratio of logistics 7, and more preferably scope is 1/3~1/2: 1.
In the inventive method, described pressure is absolute pressure.
Adopt the inventive method, select rational input and output material position in three-column process flow, and three pressure tower reasonable arrangements, namely only have smart tower III under high pressure to operate, smart tower II operation under normal pressure or pressurization, topping still I operates under negative pressure, smart tower III overhead gas can be given smart tower II tower reactor heating, and smart tower II overhead gas can be given the heating of topping still I tower reactor, and only smart tower III tower reactor needs to be heated by primary steam, realize the triple effect utilization of live steam, reduced the heating medium cost.Compared with prior art, the highest energy consumption 32.5% of saving.In addition, in the inventive method, only have tower of topping still I to contain wine with dregs, and operate under negative pressure, contain the wine with dregs portion temperature in tower low, can be low to moderate 76 ℃, and in prior art, topping still tower reactor temperature is high to 112 ℃, so adopt the inventive method can avoid the material coking and stop up column plate, obtained technique effect preferably.
Description of drawings
Fig. 1 is schematic flow sheet of the present invention.
Fig. 2 is the schematic flow sheet of document CN101085717A.
In Fig. 1, I is topping still, and II is smart tower 1, and III is that smart tower 2,1 is fermentation liquid, and 2 is thick wine, and 3 are useless grain, and 4 is the azeotropic ethanol product, and 5 is weak liquor, and 6,7 and 8 is high wine, and 9 is smart tower waste water.
In Fig. 2, IV is topping still, and V is the low pressure azeotropy rectification column, and VI is the high pressure azeotropy rectification column, 10 is fermentation liquid, and 11 are useless mash, and 12 is thick fume, and 13,15 is azeotropic ethanol, 14 is weak liquor, and 16 is smart tower waste water, and 17 is high pressure azeotropy rectification column top gaseous phase lime set.
In Fig. 1, fermentation liquid 1 enters the top of topping still I, after slightly heating up in a steamer, obtains thick wine 2 at the tower top of topping still I, obtains useless grain 3 in the tower reactor of topping still I.Thick wine 2 enters the bottom of smart tower II, after rectifying, tower top at smart tower II obtains azeotropic ethanol product 4, tower reactor at smart tower II obtains weak liquor 5, and weak liquor 5 enters the bottom of smart tower III, after rectifying, tower top at smart tower III obtains high wine 8, high wine 8 is divided into logistics 6 and logistics 7 two portions, and logistics 6 enters smart tower II top, and logistics 7 is back to smart tower III top.
In Fig. 2, fermentation liquid 10 enters the top of topping still IV, after slightly heating up in a steamer, from the thick fume 12 of topping still side line extraction gas phase, obtains useless mash 11 in the topping still tower reactor.Thick fume 12 enters low pressure azeotropy rectification column V bottom, after rectifying, from low pressure azeotropy rectification column top side line extraction azeotropic ethanol 13, obtains weak liquor 14 in low pressure azeotropy rectification column tower reactor.The lime set 17 of azeotropic alcohol 13 and high pressure azeotropy rectification column top gaseous phase is together as the phegma of high pressure azeotropy rectification column.Weak liquor 14 enters the middle part of high pressure azeotropy rectification column VI, after rectifying, from the top side line extraction azeotropic ethanol 15 of high pressure azeotropy rectification column, obtains smart tower waste water 16 in the tower reactor of high pressure azeotropy rectification column.
The present invention is further elaborated below by embodiment.
Embodiment
[embodiment 1]
Adopt flow process shown in Figure 1, ethanol content is the top that the fermentation liquid 1 of 10 % by weight enters topping still I, after slightly heating up in a steamer, obtain at the tower top of topping still I the thick wine 2 that ethanol content is 48 % by weight, obtain ethanol content less than useless poor 3 of 0.005 % by weight in the tower reactor of topping still I.Thick wine 2 enters the bottom of smart tower II, after rectifying, obtains azeotropic ethanol product 4 at the tower top of smart tower II, obtains in the tower reactor of smart tower II the weak liquor 5 that ethanol content is 40 % by weight.Weak liquor 5 enters the bottom of smart tower III, after rectifying, tower top at smart tower III obtains the high wine 8 that ethanol content forms near azeotropic, and the part (60%) 6 of high wine 8 enters the top of smart tower II, and another part 7 of high wine 8 passes back into smart tower III tower top.
The topping still stage number is 26, and feed entrance point is the 2nd block of column plate, and working pressure is 30kPa, and tower top temperature is 54 ℃, and the tower reactor temperature is 76 ℃.
Essence tower II stage number is 50, and feed entrance point is 48, and working pressure is 110kPa, and tower top temperature is 81 ℃, and the tower reactor temperature is 87 ℃.
Essence tower III stage number is 68, and feed entrance point is the 60th block of column plate, and working pressure is 350kPa, and tower top temperature is 113.2 ℃, and the tower reactor temperature is 137.3 ℃.
Do not occur the material coking in topping still and stop up the phenomenon of column plate.The steam total flow is 1.2 tons of steam/ton azeotropic ethanol product, and azeotropic ethanol product per ton is compared with [comparative example 1] and can be saved 25% energy consumption.
[embodiment 2~4]
Adopt flow process shown in Figure 1, just change the operational condition of each tower.Concrete operational condition and steam consumption see Table 1.
Table 1
Figure G2010100227479D00041
[comparative example 1]
Adopt flow process shown in Figure 2, fermentation liquid 10 enters the top of topping still IV, after slightly heating up in a steamer, from the thick fume 12 of topping still side line extraction gas phase, obtains useless mash 11 in the topping still tower reactor.Thick fume 12 enters low pressure azeotropy rectification column V bottom, after rectifying, from low pressure azeotropy rectification column top side line extraction azeotropic ethanol 13, obtains weak liquor 14 in low pressure azeotropy rectification column tower reactor.The lime set 17 of azeotropic ethanol 13 and high pressure azeotropy rectification column top gaseous phase is together as the phegma of high pressure azeotropy rectification column.Weak liquor 14 enters the middle part of high pressure azeotropy rectification column VI, after rectifying, from the top side line extraction azeotropic ethanol 15 of high pressure azeotropy rectification column, obtains smart tower waste water 16 in the tower reactor of high pressure azeotropy rectification column.
The topping still stage number is 26, and feed entrance point is the 2nd block of column plate from top to bottom, tower top working pressure 140kPa, 101 ℃ of tower top service temperatures, 112 ℃ of tower reactor service temperatures.
Low pressure azeotropy rectification column stage number is 50, and feed entrance point is the 48th block of column plate from top to bottom, tower top working pressure 110kPa, 77 ℃ of tower top service temperatures, 94 ℃ of tower reactor service temperatures.
High pressure azeotropy rectification column stage number is 68, and feed entrance point is the 35th block of column plate from top to bottom, tower top working pressure 580kPa, 128 ℃ of tower top service temperatures, tower reactor service temperature 158.
The column plate phenomenon appears in topping still stopping up.Steam consumption is 1.6 tons of steam/ton azeotropic ethanol product.

Claims (6)

1. the three-tower differential pressure distillating method of an azeotropic ethanol processed comprises the following steps:
A) fermentation liquid enters the top of topping still (I), and after slightly heating up in a steamer, tower top obtains the first logistics (2), and tower reactor obtains useless grain;
B) the first logistics (2) enters the first smart tower (II) bottom, and after rectifying, tower top obtains the product azeotropic ethanol, and tower reactor obtains the second logistics (5);
C) the second logistics (5) enters the second smart tower (III) bottom, and after rectifying, tower top obtains the 3rd logistics (8), and tower reactor obtains smart tower waste water; Wherein, described the 3rd logistics (8) is divided into the 4th logistics (6) and the 5th logistics (7) two portions, and the 4th logistics (6) enters the first smart tower (II) top, and the 5th logistics (7) is back to the second smart tower (III) top;
The working pressure P of topping still (I) IBe 20kPa<P I<50kPa, perhaps 50kPa<P I<70kPa; The working pressure of the first smart tower (II) is 100~200kPa; The working pressure of the second smart tower (III) is 350~550kPa; The working pressure of topping still (I), the first smart tower (II) and the second smart tower (III) increases successively.
2. the three-tower differential pressure distillating method of azeotropic ethanol processed according to claim 1, the operational condition that it is characterized in that topping still (I): stage number is 20~30, tower top temperature is 50~70 ℃, and the tower reactor temperature is that 70~100 ℃ of feed plate positions are positioned at from top to bottom the 2nd~10 column plate place;
The operational condition of the first smart tower (II): stage number is 40~70, and tower top temperature is 75~100 ℃, and the tower reactor temperature is 80~110 ℃, and the feed plate position is positioned at from top to bottom the 40th~50 column plate place;
The operational condition of the second smart tower (III): stage number is 50~80, and tower top temperature is 100~140 ℃, and the tower reactor temperature is 120~160 ℃; The feed plate position is positioned at from top to bottom the 55th~65 column plate place.
3. the three-tower differential pressure distillating method of azeotropic ethanol processed according to claim 2, it is characterized in that the operational condition of topping still (I): stage number is 22~28, and tower top temperature is 53~65 ℃, and the tower reactor temperature is 75~90 ℃;
The operational condition of the first smart tower (II): stage number is 50~65, and tower top temperature is 80~90 ℃, and the tower reactor temperature is 85~100 ℃;
The operational condition of the second smart tower (III): stage number is 65~75, and tower top temperature is 110~130 ℃, and the tower reactor temperature is 125~145 ℃.
4. the three-tower differential pressure distillating method of azeotropic ethanol processed according to claim 1 is characterized in that the working pressure P of topping still (I) IBe 30kPa<P I<50kPa, perhaps 50kPa<P I<60kPa.
5. the three-tower differential pressure distillating method of azeotropic ethanol processed according to claim 1, is characterized in that the 4th logistics (6) and the weight ratio of the 5th logistics (7) are 1/4~1: 1.
6. the three-tower differential pressure distillating method of azeotropic ethanol processed according to claim 5, is characterized in that the 4th logistics (6) and the weight ratio of the 5th logistics (7) are 1/3~1/2: 1.
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CN102489030A (en) * 2011-12-07 2012-06-13 肥城金塔酒精化工设备有限公司 Three-tower energy-saving differential pressure alcohol distillation production system and technological process thereof
CN104262090B (en) * 2014-09-22 2016-06-29 江苏九天高科技股份有限公司 The production method of a kind of biomass dehydrated alcohol and device
CN108613531B (en) * 2018-03-28 2020-01-14 中石化上海工程有限公司 Method for drying lactide in molten state

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Publication number Priority date Publication date Assignee Title
CN1736527A (en) * 2005-06-30 2006-02-22 广东中科天元再生资源工程有限公司 Alcohol quinque-towel differential pressure distilling arrangement and technique thereof
CN101085717A (en) * 2007-06-01 2007-12-12 蓝仁水 Method for rectifying ethanol by three-tower heat integration device
CN101580457A (en) * 2008-05-13 2009-11-18 广东中科天元新能源科技有限公司 Device and process for preparing absolute ethyl alcohol by taking fermented liquor as the raw material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1736527A (en) * 2005-06-30 2006-02-22 广东中科天元再生资源工程有限公司 Alcohol quinque-towel differential pressure distilling arrangement and technique thereof
CN101085717A (en) * 2007-06-01 2007-12-12 蓝仁水 Method for rectifying ethanol by three-tower heat integration device
CN101580457A (en) * 2008-05-13 2009-11-18 广东中科天元新能源科技有限公司 Device and process for preparing absolute ethyl alcohol by taking fermented liquor as the raw material

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