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WO1990007367A1 - Methode et appareil de purification par distillation d'un melange liquide binaire - Google Patents

Methode et appareil de purification par distillation d'un melange liquide binaire Download PDF

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Publication number
WO1990007367A1
WO1990007367A1 PCT/FI1990/000002 FI9000002W WO9007367A1 WO 1990007367 A1 WO1990007367 A1 WO 1990007367A1 FI 9000002 W FI9000002 W FI 9000002W WO 9007367 A1 WO9007367 A1 WO 9007367A1
Authority
WO
WIPO (PCT)
Prior art keywords
column
still head
liquid mixture
mixture
distillate
Prior art date
Application number
PCT/FI1990/000002
Other languages
English (en)
Inventor
Olavi LEPPÄNEN
Raimo Laakso
Original Assignee
Oy Alko Ab
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Oy Alko Ab filed Critical Oy Alko Ab
Publication of WO1990007367A1 publication Critical patent/WO1990007367A1/fr

Links

Classifications

    • 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
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/322—Reboiler specifications
    • 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
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40—Extractive distillation

Definitions

  • the present invention concerns a method for the purification of a two-component liquid mixture by distillation, in which method the liquid mixture to be purified is supplied into a multi-plate purifying column, between its bottom space and still head, a diluting liquid consisting of one of the components of the liquid mixture is fed into the column, a distillate containing volatile impurities is obtained from the still head and the purified two-component liquid mixture is obtained from the bottom of the column.
  • the invention also concerns a distillation apparatus for the purification of a two-component liquid mixture by distillation, said apparatus comprising a multi-plate purifying column; feed equipment for supply ⁇ ing the mixture to be purified into the column below the top plate; feed equipment for supplying a diluting liquid consisting of one of the components of the liquid mixture into the column; a still head outlet, with possible refluxing, for the removal of the distillate vapours from the still head; and a bottom outlet, with possible refluxing, for the removal of the bottom product from the bottom of the column.
  • the invention relates to a meth ⁇ od and an apparatus for the purification of a two-compo ⁇ nent liquid mixture by distillation, said two-component liquid mixture containing a compound with a higher boil- ing point and another compound with a lower boiling point.
  • These compounds of the liquid mixture may be any liquids permitting purification by distillation.
  • the invention concerns a method and a cor ⁇ responding apparatus for the purification of a mixture of water and ethanol in the manufacture of drinkable alcohol.
  • the alcohol is usually separated by distillation in a mash column in which raw alcohol is obtained from the still head and the grain with low alcohol content from the bottom.
  • the raw alcohol obtained from the mash column usually having an alcohol concentration of 30 - 50 % by weight, can be passed to a purifying or hydroselection column either directly in the vaporized state or in liquid state after condensation, or after it has been rectified into raw spirit, which typically has a concentration of 88 - 94 % by weight.
  • the raw alcohol or raw spirit is diluted with water and subjected to extractive distillation. During this stage, the raw alcohol is effectively purified of substances that are undesirable in clear spirit of neutral smell and taste, e.g. vodka.
  • the evaporability of the impurities increases as the ethanol content of the water-ethanol mixture decreases.
  • the rest of the impurities contained in the ethanol- water mixture obtained from the bottom of the purifying column are concentrated partly in the still head and partly in the so-called fusel zone of the rectifying column, from where they can be removed.
  • the fusel zone of the rectifying column is located in the region where the ethanol content of the ethanol-water mixture boiling on the column plates is approx. 10 - 70 % by weight.
  • a so-called methanol column is used. From this, the pure alcohol is obtained from the bottom while the fraction containing impurities, e.g. methanol, is obtained from the still head.
  • industrial extractive purifica- tion of raw alcohol can be implemented in two ways re ⁇ garding the manner in which the diluting water is sup ⁇ plied into the column.
  • the raw alco ⁇ hol and the required diluting water are fed in together onto the same plate, located several plates below the still head.
  • the purified ethanol-water mixture typical ⁇ ly having a concentration of 8-20 % by weight, is ob ⁇ tained from the bottom of the column while the undesir ⁇ able compounds are removed from the still head in the form of distillate vapour.
  • the ethanol content of the dis- tillate vapour obtained from the still head typically amounts to a value exceeding 80 % by weight.
  • the raw alcohol is fed into the column at a point below the top plate while the diluting water is supplied onto the top plate of the column.
  • the purified ethanol-water mixture typically having a concentration of 8-20 % by weight, is obtained from the bottom of the column.
  • the undesirable compounds are re ⁇ moved from the still head of the purifying column in the form of a distillate vapour which typically has an ethanol concentration below 30 % by weight.
  • the distillate vapour obtained from the still head need not be refluxed after condensation back to the top plate, because the diluting water supplied to the top plate constitutes a reflux in the upper part of the column and is responsible for the low ethanol content of the distillate vapour obtained from the still head.
  • the liquid is heated to a boiling temperature by means of steam either directly by supplying it into the bottom space of the column or indirectly using a heat exchanger.
  • the purifying column typically needs 1 - 3
  • the object of the invention is to achieve a method and an apparatus for implementing purifiying distillation in such a way as to reduce the energy required for the distillation to a level essentially below the energy requirement of previously known methods and apparatuses.
  • the present invention provides a new and sur ⁇ prising solution regarding the energy requirement of the purifying column.
  • the heat content of the vapour obtained from the still head of the purifying column can be utilized for the heating of the bottom space of the same column.
  • the vapour obtained from the still head of the purifying column need not be compressed mechanically or by other means to increase its temperature.
  • the mixture itself or one of its compo- nents e.g. the one with the lower boiling point
  • the other component e.g. a diluting liquid having a higher boiling point
  • the supply of the diluting liquid and the operational conditions in the column are adjusted as described below so as to ensure that the temperature in the still head is higher than the temperature at the bottom of the column.
  • the vapour obtained from the still head can be used for the heating of the bottom space.
  • the apparatus of the invention comprises equip ⁇ ment for supplying a diluting liquid onto the top plate, below the top plate or both onto and below the top plate, and equipment for supplying the liquid mixture to be purified into the purifying column at a point below the point of supply of the diluting liquid.
  • the novelty in the apparatus of the invention is its equipment for passing part of the heat content of the distillate vapour obtained from the still head into the bottom space of the column e.g. by means of a heat exchanger serving to maintain a boiling temperature in the bottom space.
  • the boiling tem ⁇ perature of the liquid at the bottom was always dis ⁇ tinctly higher than the temperature of the distillate vapour obtained from the top of the column because the liquid at the bottom has a lower ethanol content and a higher pressure than the distillate vapour obtained from the top.
  • the second operational mode of the purifying column by varying the amount of diluting liquid used, the position of the point of supply of raw alcohol in the column and the intensity of the boiling, it is possible to exert a strong influence on the temperature of the distillate vapour removed from the top of the column and, to a lesser extent, on the boiling point of the liquid at the bottom of the column.
  • the purifying column has 25 - 50 bubble, sieve or valve plates, across which the pressure loss in the column during distillation is usually 75 - 250 mbar. If packed column fillers with a small pressure loss are used, the pressure difference in the column can be kept at a level below 50 mbar.
  • the distillate vapour obtained from the still head of the purifying column is passed essentially as such and directly from the still head to the secondary side of a heat exchanger communicating with the bottom space of the same column, in such manner that the distillate vapour is partly or completely condensed in the exchanger, which transfers the condensation energy of the vapour to the bottom space for use in the boiling of the liquid.
  • the arrangement provided by the invention makes it possible to achieve a substantial reduction in the amount of external energy required by the purifying column.
  • the apparatus of the invention can also be used for the purifying distillation of raw alcohol or impure spirit produced in other ways besides fermentation, e.g. synthetic spirit.
  • the alcohol to be purified has a concentration of e.g. 20 - 90 % by weight.
  • the alcohol to be purified is raw alcohol obtained from a mash column and has a concentration of 35 - 50 % by weight.
  • the alco ⁇ hol to be purified is raw alcohol with a concentration of e.g. 88 - 94 % by weight.
  • the method and apparatus of the invention are also applicable for the purification of other liquid pairs besides water-ethanol mixtures.
  • Such liquid pairs may consist e.g. of water and other kinds of alcohol, water and other organic liquids, and/or organic liquids in general.
  • Fig. 1 presents a flow- chart illustrating the operation of an industrial-scale distillation apparatus representing the state of the art.
  • Fig. 2 presents a flow chart representing an embodiment of the method and apparatus of the invention.
  • Example 1
  • a purifying column as illus- trated by Fig. 1 was used.
  • the column was a 45-plate bubble plate column.
  • Raw alcohol e.g. the distillate obtained from a mash column
  • the raw alcohol feed can be preheated in some other heat exchanger belonging to the distillation system.
  • the purified weak alcohol solution typically having an ethanol content of 8 - 20 % by weight, was passed from the bottom space 6 via output line 7 to other parts of the distillation system for further processing.
  • the ethanol-containing vapour obtained from the still head 5 of the purifying column is passed via line 4 into a heat exchanger 12, where it is condensed.
  • the condensed vapour, the so-called distillate was removed from the heat exchanger via line 10 and directed to other parts of the distillation system for further processing.
  • the apparatus was provided with another heat exchanger 8 connected to the bottom space of the column. Via line 10, primary vapour was supplied to the primary side of the heat exchanger.
  • the condensed vapour, the so-called primary condensate was removed from the heat exchanger via exhaust line 11 and passed to other parts of the distillation system for further processing.
  • the heat energy released in the condensation of the primary vapour was transferred to the secondary side of the heat exchanger and further via line 9 to the bottom space of the purifying column, causing the liquid in the bottom space to boil.
  • thermal power fed into heat exchanger 8 in example 1 can be calculated as follows:
  • the distillate vapour flow 4 Since the distillate vapour flow 4 has an etha ⁇ nol content of 2.64 % by weight, the temperature falls in the total condensation from 105°C to 101.9"C. Since the condensation temperature in the total condensation is higher than the temperature in the bottom space of the purifying column in example 1, the distillate vapour can be directed to a heat exchanger providing heat for the boiling of the liquid in the bottom space as illus ⁇ trated by Fig. 2, thus enabling the entire condensation heat to be transferred to the bottom space to maintain the boiling temperature.
  • Example 2 shows that the method and apparatus of the invention enable the required external boiling energy of the purifying column to be reduced from a value of 2627 MJ/h to a value of 200 MJ/h.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Méthode de purification par distillation d'un mélange de liquide binaire, par laquelle le mélange liquide à purifier passe dans une colonne de purification multiplaque entre son espace de fond et le chapiteau de la cucurbite, le liquide diluant constitué de l'un des composants du mélange liquide est introduit dans la colonne, un distillat renfermant des impuretés volatiles est obtenu au niveau du chapiteau de la cucurbite et le mélange liquide binaire purifié est obtenu au fond de la colonne, au moins une partie de la chaleur contenue dans le distillat obtenu dans le chapiteau de la cucurbite étant dirigée vers l'espace du fond de la colonne, par exemple, en faisant passer le distillat à travers un échangeur de chaleur qui transfère de la chaleur à l'espace du fond.
PCT/FI1990/000002 1988-12-30 1990-01-02 Methode et appareil de purification par distillation d'un melange liquide binaire WO1990007367A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI886052 1988-12-30
FI886052A FI80218C (fi) 1988-12-30 1988-12-30 Foerfarande och anlaeggning foer rening av en tvaokomponentvaetskeblandning medelst destillering.

Publications (1)

Publication Number Publication Date
WO1990007367A1 true WO1990007367A1 (fr) 1990-07-12

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/FI1990/000002 WO1990007367A1 (fr) 1988-12-30 1990-01-02 Methode et appareil de purification par distillation d'un melange liquide binaire

Country Status (4)

Country Link
EP (1) EP0456647A1 (fr)
AU (1) AU4822390A (fr)
FI (1) FI80218C (fr)
WO (1) WO1990007367A1 (fr)

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US8884079B2 (en) 2011-08-03 2014-11-11 Celanese International Corporation Reducing impurities in hydrogenation processes with multiple reaction zones
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SE193714C1 (fr) * 1961-05-08 1965-01-05 Shell Oil Company
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EP0043023A1 (fr) * 1980-06-27 1982-01-06 Raphael Katzen Associates International, Inc. Procédé et appareillage pour la distillation d'alcool hydraté
EP0203259A2 (fr) * 1985-02-06 1986-12-03 Linde Aktiengesellschaft Procédé de régénération d'un produit de lavage chargé
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SE193713C1 (fr) * 1961-04-14 1965-01-05 Shell Internationale Research Maatschappij Nv
SE193714C1 (fr) * 1961-05-08 1965-01-05 Shell Oil Company
SE361824B (fr) * 1968-03-26 1973-11-19 Treadwell Corp
DE2340566A1 (de) * 1973-08-10 1975-02-27 Peter Siegfried Verfahren zur trennung von stoffgemischen durch extraktive destillation
EP0043023A1 (fr) * 1980-06-27 1982-01-06 Raphael Katzen Associates International, Inc. Procédé et appareillage pour la distillation d'alcool hydraté
SE451846B (sv) * 1981-09-23 1987-11-02 N Proizv Gidroliznoe Ob Meskrektificeringsanordning samt forfarande for automatisk styrning av densamma
EP0203259A2 (fr) * 1985-02-06 1986-12-03 Linde Aktiengesellschaft Procédé de régénération d'un produit de lavage chargé

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1459794A2 (fr) 2003-03-18 2004-09-22 Nippon Shokubai Co., Ltd. Dispositif et procédé de purification de l'acide acrylique et membres de la famille
EP1459794A3 (fr) * 2003-03-18 2004-10-20 Nippon Shokubai Co., Ltd. Dispositif et procédé de purification de l'acide acrylique et membres de la famille
US7014736B2 (en) 2003-03-18 2006-03-21 Nippon Shokubai Co., Ltd. Apparatus and process for purification of acrylic acid family
US9447005B2 (en) 2010-02-02 2016-09-20 Celanese International Corporation Processes for producing anhydrous ethanol compositions
US8884079B2 (en) 2011-08-03 2014-11-11 Celanese International Corporation Reducing impurities in hydrogenation processes with multiple reaction zones

Also Published As

Publication number Publication date
AU4822390A (en) 1990-08-01
FI80218C (fi) 1990-05-10
EP0456647A1 (fr) 1991-11-21
FI80218B (fi) 1990-01-31

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