CN101367710A - Process and apparatus for preparing absolute ethyl alcohol - Google Patents
Process and apparatus for preparing absolute ethyl alcohol Download PDFInfo
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- CN101367710A CN101367710A CNA2008101400576A CN200810140057A CN101367710A CN 101367710 A CN101367710 A CN 101367710A CN A2008101400576 A CNA2008101400576 A CN A2008101400576A CN 200810140057 A CN200810140057 A CN 200810140057A CN 101367710 A CN101367710 A CN 101367710A
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Abstract
The invention relates to a novel azeotropic distillation process method and a device thereof, in particular to a process method which use a septal azeotropic distillation column (5) to produce absolute alcohol, and a device thereof. The septal azeotropic distillation column (5) is achieved by arranging a septal wall (6) in the azeotropic distillation column in the vertical direction, and the septal wall (6) divides the space of the azeotropic distillation column into three areas with different functions; a public distillation part (1), a dehydration part (2) and a side stripper part (3). The alcohol solution to be separated is filled to the azeotropic distillation column from the upper part of the dehydration part (2), and the absolute alcohol is obtained at the bottom of the dehydration part (2); ternary azeotrope is steamed out of the top of the column, and condensed by a condenser (7) and then splitted into light phase solution and heavy phase solution in a phase splitter; the light phase solution (entrainer) reflows and the heavy phase solution is the feed stock in the side stripper part (3), and little water containing alcohol is obtained at the bottom of the side stripper part (3). The device and the process method of the invention can produce the absolute alcohol, and can simplify the process, reduce the energy consumption and the cost of the divices.
Description
Technical field
The present invention relates to a kind of processing method and device of producing dehydrated alcohol, specifically be meant a kind of processing method and device thereof that utilizes azeotropic distillation next door tower to produce dehydrated alcohol, ethanol azeotropy rectification column, entrainment agent recovery tower can be integrated in the same tower.
Background technology
Dehydrated alcohol is a kind of common chemical raw material, not only in industry such as electronics, space flight important use is arranged, and makes solvent at aspects such as medicine, agricultural chemicals and grease leachings, and dehydrated alcohol is mixed the fuel that (being commonly called as gasohol) can be used as oil engine with gasoline.Some country has determined gasohol as power fuel in the world, along with the minimizing of world petroleum resource, may occupy a tiny space in power fuel from now on as the dehydrated alcohol of biofuel.In addition, also can be used as the raw material (be with benzene entrainment agent except) and the chemical reagent of superior cosmetics.
At present, the common method of production dehydrated alcohol has extractive distillation method, ion-exchange-resin process, azeotropic distillation.In the extractive distillation method, the recovery of lyonium salt is a problem that awaits solving.And ion-exchange-resin process can only be used for batch production, and have that output is little, defective such as energy consumption is big, regeneration difficulty, ethanol loss and labour intensity are big.Production is continuous, mechanization degree is high, the consumes energy grade is low, the product purity advantages of higher because azeotropic distillation has, and is the main method of suitability for industrialized production dehydrated alcohol therefore.
U.S. Pat 4256541 provides a kind of production method of dehydrated alcohol: device is by a stripping tower, a rectifying tower, a dehydration tower, and a phase splitter and other auxiliary facilitys are formed.The aqueous ethanolic solution of lower concentration enters rectifying tower rectifying after the stripping tower stripping, enter dehydration tower and under high pressure utilize cyclohexane give to carry out azeotropic distillation for entrainment agent through carrying the dense aqueous ethanolic solution that obtains, and obtains the dehydrated alcohol product at the bottom of tower.Dehydration column overhead is provided with a phase splitter, gently refluxes mutually, and heavy phase is returned and entered rectifying tower.This technical process complexity, the facility investment expense is higher.
U.S. Pat 4422903 provides one to overlap the product (the ethanol mass content is 0.5%～20%) that utilizes carbohydrate fermentation and obtain is produced dehydrated alcohol as raw material device: this device is made up of a stripping tower, a rectifying tower, a dehydration tower, an entrainment agent recovery tower and other auxiliary facilitys.Raw material enters rectifying tower after the stripping tower stripping, after being improved, the rectifying alcohol concn enters dehydration tower, in dehydration tower, utilize benzene to carry out azeotropic distillation as entrainment agent, obtain the dehydrated alcohol product at the bottom of the tower, the gas phase of cat head is divided into the weight two-phase after separating, gently reflux mutually, the entrainment agent that utilizes the entrainment agent recovery tower to reclaim in the heavy phase reuses.This technological operation is comparatively complicated, and facility investment and energy consumption are higher.
Chinese patent CN 200410064085.0 provides the production of fuel ethanol method: the azeotropic ethanol gas phase that adopts distillating method to obtain obtains anhydrous process of alcohol products behind molecular sieve dehydration.Distallation systm is made up of wine with dregs tower and 2 towers of dehydration tower, and also need pass through molecular sieve dehydration, has energy consumption height, shortcoming that output is little.
Chinese patent CN 200610035950.3 provides a kind of fuel alcohol dewatering apparatus: rectifying tower that having adopted connects is provided with and stripping tower, two molecular sieves, superheater, reactor product cooler, the feed preheater that are arranged in parallel.Though this device can be realized the recycling of heat, production process is pollution-free, whole flow process complexity, energy consumption height.
Chinese patent CN 02148634.4 provides a kind of raw materials for production liquid (the ethanol mass content is 5%～30%) that utilizes to produce ultrapure ethanol for raw material, this production equipment mainly is made up of topping still, dealdehyder tower, treating tower, eparating methanol tower and recovery tower, the advantage of this technology is: dealdehyder tower and treating tower are tray column and packing tower composite structure, dealdehyder tower is realized once ester class, aldehydes and fusel wet goods impurity being carried out whole removal of impurities, and rectifying tower is realized the whole removal of impurities for the second time of impurity such as potato spirit and aldehydes.But whole process flow complexity, energy consumption height.
Conventional aqueous ethanolic solution azeotropic distillation device is two tower flow processs, comprises an ethanol azeotropy rectification column and an entrainment agent recovery tower.Azeotropic distillation next door tower then is that the azeotropic distillation process is applied in the tower of next door, finishes the task such as separation, entrainment agent recovery of second alcohol and water in a tower simultaneously.Than two tower azeotropic distillation flow processs of routine, a rectifying tower and a condenser have been saved.Therefore and azeotropic distillation next door tower can effectively be avoided the back-mixing effect in the old process, and thermodynamic(al) efficiency is higher, can cut down the consumption of energy effectively and reduces facility investment, increases economic efficiency.
Summary of the invention
The purpose of this invention is to provide a kind of processing method and device that utilizes azeotropic distillation next door tower to produce dehydrated alcohol.The present invention reclaims separation, the entrainment agent of second alcohol and water to be integrated in the same tower, can directly obtain dehydrated alcohol, has simplified conventional azeotropic distillation flow process, has reduced energy consumption and facility investment effectively.
Device of the present invention is an azeotropic distillation next door tower (5), a next door (6) that extends to tower top from tower bottom promptly is set on the vertical direction in the conventional rectification tower, next door (6) is divided into three zones with space in azeotropic distillation next door tower (5) tower, wherein zone (1) is public rectifying section, zone (2) is a dewatering period, and zone (3) is the side line stripping section.Next door (6) is that off-centre or center are provided with, and dewatering period (2) is 3:1～1:1 with the cross-sectional area ratio of side line stripping section (3).Azeotropic distillation next door tower (5) can be tray column, packing tower or both arbitrary combination.
Method of the present invention is: aqueous ethanolic solution is replenished entrainment agent and is added by phase splitter (4) by dewatering period (2) top charging.In public rectifying section (1), because the effect of entrainment agent, the azeotropic system of second alcohol and water is broken, form new ternary azeotrope, ethanol, water and entrainment agent ternary azeotrope steam from cat head, are divided into weight two-phase liquid after condenser (7) condensation in phase splitter (4), gently reflux mutually, heavy phase is sent into the top of side line stripping section (3), as the charging of side line stripping section (3).(6) top inflow dewatering period (2) is 15:1～5:1 with the ratio of the liquid mass flow of side line stripping section (3) from the next door.Obtain the dehydrated alcohol product in dewatering period (2) bottom, obtain containing the water of small amount of ethanol in side line stripping section (3) bottom.The used entrainment agent of the present invention is a kind of in hexanaphthene, benzene and the pentamethylene etc.In operating process, tower top temperature is 45～110 ℃, and dewatering period (2) tower still temperature is 70～130 ℃, and side line stripping section (3) tower still temperature is 90～155 ℃, and the temperature of phase splitter (4) is 20～50 ℃.The working pressure of tower is 0.05～0.5MPa.
Obtain dehydrated alcohol product (ethanol massfraction content is more than 99.5%) among the present invention at the bottom of the tower, the entrainment agent recycle, the dehydrated alcohol product institute energy requirement that obtains same purity saves 20～40% than conventional azeotropic distillation flow process, and can save facility investment.
Description of drawings
Fig. 1 is an azeotropic distillation next door tower schematic flow sheet.
Fig. 2 is conventional azeotropic distillation schematic flow sheet.
Among the figure, 1 is public rectifying section, and 2 is dewatering period, and 3 is the side line rectifying section, and 4,12 is phase splitter, and 5 is azeotropic distillation next door tower, and 6 is the next door, and 7,13,14 is condenser, and 10 is dehydration tower, and 11 is concentration tower, and 8,9,15,16 is reboiler.
Specific embodiments
The invention will be further described by means of embodiment below, but the present invention is not limited to embodiment.
Example 1: flow process as shown in Figure 1.Azeotropic distillation next door tower (5) is that a diameter is 1000mm, highly is the tray column of 31000mm.Wherein public rectifying section (1) stage number is 5, and dewatering period (2) stage number is 60, and side line stripping section (3) stage number is 54.Dewatering period (2) is 1.38:1 with the ratio of the cross-sectional area of side line stripping section (3), and the liquid mass throughput ratio that enters dewatering period (2) and side line stripping section (3) is 12.11:1.Be entrainment agent with the hexanaphthene in this example, feed ethanol aqueous solution feed entrance point (is counted from top to bottom, be the 8th block of column plate of dewatering period (2) down together), the heavy phase backflow feed entrance point in the phase splitter (4) is the 1st a block of column plate of side line stripping section (3), replenishes entrainment agent and adds from phase splitter (4).Tower top temperature is 62.8 ℃, and pressure is 0.1MPa, and dewatering period (2) tower still temperature is 78.6 ℃, and side line stripping section (3) tower still temperature is 98.1 ℃, and phase splitter (4) temperature is 25.0 ℃.Each logistics flux and form as shown in table 1.
Table 1 example 1 each logistics quality flow and each constituent mass mark
| Extraction/charging position | Mass rate/(kg/h) | Ethanol/% | Water/% | Hexanaphthene % |
| The aqueous ethanolic solution charging replenishes the extraction of entrainment agent charging dewatering period (2) tower still extraction side line section (3) tower still | 1000 2 900 102 | 90 0 99.8 2 | 10 0 0 98 | 0 1 0.2 0 |
Example 2: flow process as shown in Figure 1.Azeotropic distillation next door tower (5) is that a diameter is 1200mm, highly be tower tray and the filler mixing column of 30000mm, wherein public rectifying section (1) uses filler, bed stuffing height is 1000mm, dewatering period (2) uses column plate with side line stripping section (3), wherein dewatering period (2) stage number is 60, and side line stripping section (3) stage number is 54.Dewatering period (2) is 1.31:1 with the ratio of the cross-sectional area of side line stripping section (3), and the liquid mass throughput ratio that enters dewatering period (2) and side line stripping section (3) is 10.60:1.Feed heat state, feed composition, feed rate are with example 1, and entrainment agent still is a hexanaphthene, and just feed entrance point changes to some extent, and feed entrance point is the 10th a block of column plate of dewatering period (2), each logistics flux and form as shown in table 2.Tower top temperature is 67.8 ℃, and pressure is 0.12MPa, and dewatering period (2) tower still temperature is 83.7 ℃, and side line stripping section (3) tower still temperature is 104.8 ℃, and the temperature of phase splitter (4) is 25.0 ℃.
Table 2 example 2 each logistics quality flow and each constituent mass mark
| Extraction/charging position | Mass rate/(kg/h) | Ethanol/% | Water/% | Hexanaphthene % |
| The aqueous ethanolic solution charging replenishes the extraction of entrainment agent charging dewatering period (2) tower still extraction side line section (3) tower still | 1000 2 900 102 | 90 0 99.7 2.6 | 10 0 0.1 97.4 | 0 1 0.2 0 |
Example 3: flow process as shown in Figure 1.Azeotropic distillation next door tower (5) is that a diameter is 1000mm, highly is the tray column of 31000mm.Wherein public rectifying section (1) stage number is 5, and dewatering period (2) stage number is 60, and side line stripping section (3) stage number is 54.Dewatering period (2) is 1.57:1 with the ratio of the cross-sectional area of side line stripping section (3), and the liquid mass throughput ratio that enters dewatering period (2) and side line stripping section (3) is 8.80:1.Feed heat state, feed rate are with example 1, and entrainment agent still is a hexanaphthene, and just the ethanol content in the charging becomes 92% (massfraction), and feed entrance point is the 12nd a block of column plate of dewatering period (2), each logistics flux and form as shown in table 3.Tower top temperature is 68.5 ℃, and pressure is 0.12MPa, and dewatering period (2) tower still temperature is 85.0 ℃, and side line stripping section (3) tower still temperature is 104.5 ℃, and the temperature of phase splitter (4) is 25.0 ℃.
Table 3 example 3 each logistics quality flow and each constituent mass mark
| Extraction/charging position | Mass rate/(kg/h) | Ethanol/% | Water/% | Hexanaphthene/% |
| The aqueous ethanolic solution charging replenishes the extraction of entrainment agent charging dewatering period (2) tower still extraction side line section (3) tower still | 1000 2 920 82 | 92 0 99.6 4.3 | 8 0 0.2 95.7 | 0 1 0.2 0 |
Example 4: flow process as shown in Figure 1.Azeotropic distillation next door tower (5) is that a diameter is 1200mm, highly is the packing tower of 26000mm.Wherein public rectifying section (1) bed stuffing height is 2000mm, and the bed stuffing height of dewatering period (2) and side line stripping section (3) is 21000mm.Dewatering period (2) is 1.34:1 with the ratio of the cross-sectional area of side line stripping section (3), and the liquid mass throughput ratio that enters dewatering period (2) and side line stripping section (3) is 6.25:1.Feed heat state, feed rate, feed composition, feed entrance point be with example 1, with benzene as entrainment agent, each logistics flux and form as shown in table 4.Tower top temperature is 64.8 ℃, and pressure is 0.1MPa, and dewatering period (2) tower still temperature is 78.6 ℃, and side line stripping section (3) tower still temperature is 100.6 ℃, and the temperature of phase splitter (4) is 25.0 ℃.
Table 4 example 4 each logistics quality flow and each constituent mass mark
| Extraction/charging position | Mass rate/(kg/h) | Ethanol/% | Water/% | Benzene/% |
| The aqueous ethanolic solution charging replenishes the extraction of entrainment agent charging dewatering period (2) tower still extraction side line section (3) tower still | 1000 2 920 82 | 92 0 99.5 5.6 | 8 0 0.3 94.2 | 0 1 0.2 0.2 |
Claims (7)
1. a device of producing dehydrated alcohol comprises azeotropic distillation next door tower (5), condenser (7), reboiler (8,9), phase splitter (4) and other utility appliance.Azeotropic distillation next door tower (5) inside is provided with a vertical next door (6), and next door (6) extend to the top of tower from the bottom of tower.Next door (6) is divided into three zones with space in azeotropic distillation next door tower (5) tower, and wherein zone (1) is public rectifying section, and zone (2) is a dewatering period, and zone (3) is the side line stripping section.
2. device as claimed in claim 1 is characterized in that next door (6) is provided with for the center or eccentric the setting, makes the dewatering period (2) and the cross-sectional area ratio of side line stripping section (3) be 3:1～1:1.
3. device as claimed in claim 1 is characterized in that azeotropic distillation next door tower (5) can be tray column, packing tower or both arbitrary combination.
4. processing method of producing dehydrated alcohol specifically may further comprise the steps:
A) raw material (aqueous ethanolic solution) replenishes entrainment agent by phase splitter (4) charging by dewatering period (2) top charging.
B) ternary azeotrope of ethanol, water and entrainment agent formation steams from cat head, is divided into weight two-phase liquid after condenser (7) condensation in phase splitter (4).
C) the light phase liquid (being rich in entrainment agent) that obtains in the phase splitter (4) enters public rectifying section (1) recycle.Heavy phase is sent into the top of side line stripping section (3), as the charging of side line stripping section (3).
D) obtain the dehydrated alcohol product in the bottom of dewatering period (2), obtain containing the water of small amount of ethanol in side line stripping section (3) bottom.
5. processing method as claimed in claim 4 is characterized in that entrainment agent is a kind of in hexanaphthene, benzene and the pentamethylene etc.
6. processing method as claimed in claim 4 is characterized in that the ratio that from the next door (6) top flows into dewatering period (2) and the liquid mass flow of side line stripping section (3) is 15:1～5:1.
7. processing method as claimed in claim 4 is characterized in that tower top temperature is 45～110 ℃, and dewatering period (2) tower still temperature is 70～130 ℃, and side line stripping section (3) tower still temperature is 90～155 ℃, and the temperature of phase splitter (4) is 20～50 ℃.The working pressure of tower is 0.05～0.5MPa.
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| CNA2008101400576A CN101367710A (en) | 2008-09-18 | 2008-09-18 | Process and apparatus for preparing absolute ethyl alcohol |
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| CN101700916B (en) * | 2009-11-06 | 2011-11-09 | 清华大学 | Process and system for treating industrial normal propyl alcohol waste liquor |
| CN102719282A (en) * | 2012-07-03 | 2012-10-10 | 华东理工大学 | Ethanol-water separation method based on automotive fuel and with methyl tertiary butyl ether (MTBE) serving as entrainer |
| CN101798528B (en) * | 2010-01-22 | 2013-02-06 | 天津大学 | Partial energy coupled separation system of carbon 3, carbon 4 and carbon 5 used in predepropanization ethylene process and operation method |
| WO2014004966A2 (en) * | 2012-06-29 | 2014-01-03 | Gevo, Inc. | Method for purification of alcohols |
| CN104649862A (en) * | 2015-02-05 | 2015-05-27 | 天津大学 | Method and equipment for producing ethanol product by taking ethyl acetate as raw material |
| CN105339062A (en) * | 2013-02-21 | 2016-02-17 | Gtc科技美国有限责任公司 | Separation processes using divided columns |
| CN106495989A (en) * | 2016-09-27 | 2017-03-15 | 广西罗城科潮基业科技发展有限公司 | A kind of alcohol of energy-conservation slightly evaporates equipment and its slightly evaporates method |
| CN106582053A (en) * | 2017-01-16 | 2017-04-26 | 天津市新天进科技开发有限公司 | Ethanol by-production process method and apparatus for partition plate tower type methanol recovery tower |
| CN106748758A (en) * | 2016-12-21 | 2017-05-31 | 常州大学 | Heat pump partition wall reactive distillation column prepares the device of isopropyl acetate |
| CN107638709A (en) * | 2016-07-27 | 2018-01-30 | 中国石化仪征化纤有限责任公司 | The separator and its operating method of acetic acid and water |
| CN108543324A (en) * | 2018-04-25 | 2018-09-18 | 四川子仁制药有限公司 | Andrographolide production alcohol recycle recycling equipment and its application method |
| CN108976115A (en) * | 2017-06-05 | 2018-12-11 | 中国石油化工股份有限公司 | A kind of method and system of separating benzene-cyclohexane and acetic acid |
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| CN101700916B (en) * | 2009-11-06 | 2011-11-09 | 清华大学 | Process and system for treating industrial normal propyl alcohol waste liquor |
| CN101798528B (en) * | 2010-01-22 | 2013-02-06 | 天津大学 | Partial energy coupled separation system of carbon 3, carbon 4 and carbon 5 used in predepropanization ethylene process and operation method |
| WO2014004966A2 (en) * | 2012-06-29 | 2014-01-03 | Gevo, Inc. | Method for purification of alcohols |
| WO2014004966A3 (en) * | 2012-06-29 | 2014-04-10 | Gevo, Inc. | Method for purification of alcohols |
| CN102719282A (en) * | 2012-07-03 | 2012-10-10 | 华东理工大学 | Ethanol-water separation method based on automotive fuel and with methyl tertiary butyl ether (MTBE) serving as entrainer |
| CN105339062A (en) * | 2013-02-21 | 2016-02-17 | Gtc科技美国有限责任公司 | Separation processes using divided columns |
| CN105339062B (en) * | 2013-02-21 | 2021-03-26 | Gtc科技美国有限责任公司 | Separation process using divided column |
| CN104649862A (en) * | 2015-02-05 | 2015-05-27 | 天津大学 | Method and equipment for producing ethanol product by taking ethyl acetate as raw material |
| CN107638709A (en) * | 2016-07-27 | 2018-01-30 | 中国石化仪征化纤有限责任公司 | The separator and its operating method of acetic acid and water |
| US10399004B2 (en) | 2016-09-08 | 2019-09-03 | Eastman Chemical Company | Thermally integrated distillation systems and processes using the same |
| US10835837B2 (en) | 2016-09-08 | 2020-11-17 | Eastman Chemical Company | Thermally integrated distillation systems and processes using the same |
| CN106495989A (en) * | 2016-09-27 | 2017-03-15 | 广西罗城科潮基业科技发展有限公司 | A kind of alcohol of energy-conservation slightly evaporates equipment and its slightly evaporates method |
| CN106748758A (en) * | 2016-12-21 | 2017-05-31 | 常州大学 | Heat pump partition wall reactive distillation column prepares the device of isopropyl acetate |
| CN106582053A (en) * | 2017-01-16 | 2017-04-26 | 天津市新天进科技开发有限公司 | Ethanol by-production process method and apparatus for partition plate tower type methanol recovery tower |
| CN106582053B (en) * | 2017-01-16 | 2019-06-14 | 天津市新天进科技开发有限公司 | The process and device of the tower methanol distillation column by-product ethyl alcohol of partition |
| CN108976115A (en) * | 2017-06-05 | 2018-12-11 | 中国石油化工股份有限公司 | A kind of method and system of separating benzene-cyclohexane and acetic acid |
| CN108543324A (en) * | 2018-04-25 | 2018-09-18 | 四川子仁制药有限公司 | Andrographolide production alcohol recycle recycling equipment and its application method |
| CN111467824A (en) * | 2020-03-31 | 2020-07-31 | 陕西聚能新创煤化科技有限公司 | Device and method for treating coal-to-liquid byproduct fusel by using partition plate rectifying tower |
| CN111467824B (en) * | 2020-03-31 | 2023-08-25 | 陕西聚能新创煤化科技有限公司 | Device and method for treating coal-to-liquid by-product fusel through baffle rectifying tower |
| CN111675601A (en) * | 2020-05-09 | 2020-09-18 | 雅邦绿色过程与新材料研究院南京有限公司 | Novel process and device for separating and purifying industrial ethanol |
| CN111675601B (en) * | 2020-05-09 | 2023-04-07 | 雅邦绿色过程与新材料研究院南京有限公司 | Novel process and device for separating and purifying industrial ethanol |
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