FI80218C - Process and plant for purification of a two-component liquid mixture by distillation - Google Patents

Process and plant for purification of a two-component liquid mixture by distillation Download PDF

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Publication number
FI80218C
FI80218C FI886052A FI886052A FI80218C FI 80218 C FI80218 C FI 80218C FI 886052 A FI886052 A FI 886052A FI 886052 A FI886052 A FI 886052A FI 80218 C FI80218 C FI 80218C
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Finland
Prior art keywords
column
liquid mixture
purification
distillation
distillate
Prior art date
Application number
FI886052A
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Finnish (fi)
Swedish (sv)
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FI80218B (en
Inventor
Olli Leppaenen
Raimo Laakso
Original Assignee
Alko Ab Oy
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Publication date
Application filed by Alko Ab Oy filed Critical Alko Ab Oy
Priority to FI886052A priority Critical patent/FI80218C/en
Priority to FI886052 priority
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Publication of FI80218B publication Critical patent/FI80218B/en
Publication of FI80218C publication Critical patent/FI80218C/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/322Reboiler specifications
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/001Processes specially adapted for distillation or rectification of fermented solutions
    • B01D3/003Rectification of spirit
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40Extractive distillation

Description

! 80218

METHOD AND APPARATUS FOR PURIFYING A TWO-COMPONENT LIQUID MIXTURE BY DISTILLATION

The present invention relates to a process for purifying a two-component liquid mixture from impurities by distillation, in which the liquid mixture to be purified is fed to a multi-bottomed purification column between the bottom space and the top, the liquid component is fed to .

The invention further relates to a distillation apparatus for purifying a two-component liquid mixture from impurities by distillation, the apparatus comprising a multi-bottomed purification column; feeders for feeding the mixture to be cleaned below the top base; feeders for passing the second component of the liquid mixture to the purification column as a diluent; 20 peak removal, equipped with a possible recovery to remove distillate vapors from the top of the column; and removing the bottom, optionally provided with a return, to remove the bottom product from the bottom of the column.

In particular, the invention relates to a method and apparatus for purifying a two-component liquid mixture by distillation, the two-component liquid mixture containing an upper-boiling compound and a lower-boiling second compound. The compounds of the liquid pair can be any of 30 liquid pairs of liquids to be purified by distillation.

In particular, the invention relates to a method and corresponding apparatus for purifying a water-ethanol mixture in connection with the preparation of potable alcohol.

In the preparation of potable alcohol, the alcohol is usually separated from the fermented 35 mash by distillation using a mash column with crude alcohol removed from the top and an alcohol-poor rank from the bottom. Depending on the distillation system used, the crude alcohol to be removed from the mash column, typically at a concentration of 30 to 50% by weight, can be passed directly as a vapor or liquid after condensation to a purification column or concentrated to a crude alcohol of a concentration of -%, before passing to the hydroselection column.

In the purification column, the crude alcohol or alcohol is diluted with water and an extractive distillation step is performed. This extractive distillation effectively removes impurities from the crude alcohol that are undesirable in clear, neutrally odorous and flavored alcohols such as vodka.

Unwanted impurities typically include sicotanic alcohols, aldehydes, esters, and other low concentrations of organic compounds in the crude alcohol. The volatility of impurities relative to ethanol increases as the ethanol content of the water-ethanol mixture decreases. In order to achieve the necessary reduction in ethanol content in the purification column, water is fed to dilute the crude alcohol or alcohol in the distillation step. Due to the aqueous dilution, the relative volatility of the undesired compounds rises sharply, causing them to be enriched to the top of the column, from which they can be removed as a so-called pre-distillate. The purified, dilute alcoholic solution to be removed from the bottom of the purification column is passed to a concentration column included in the distillation system for reconcentration. Concentrated alcohol is obtained from the top of the concentrated column and alcohol-poor water, so-called tap water, is obtained from the bottom space, which can be reused as dilution water for the purification column. The remaining impurities that have passed through the ethanol-water mixture through the bottom of the purification column are enriched partly to the top of the concentration column and partly to the so-called piglet zone of the 35 concentration column, from which they can be removed. The pig zone of the concentration column is located in an area where the ethanol content of the 11,380,218 ethanol-water mixture boiling at the bottom of the column is about 10-70% by weight.

In order to increase the quality of the concentrated alcohol distillate obtained from the concentration column, the so-called a methanol column from the bottom to give 5 pure alcohol and from the top a fraction containing impurities such as methanol.

Industrially, the extractive distillation of crude alcohol can in principle be carried out in two ways, considering the method of feeding the dilution water to the purification column. According to the first method, the crude alcohol and the required dilution water are fed together several bottoms below the top of the column to the same distillation bottom. A purified ethanol-water mixture, typically at a concentration of 8-15% by weight, is removed from the bottom of the column. Unwanted compounds are removed from the top of the purification column as distillate vapor. Since the feed bottom or bottoms of the column are below the top bottom, a portion of the ethanol-containing steam removed from the top of the column is returned to the top bottom of the column 20 after condensation to operate the top of the column. As a result of the recovery, the ethanol content of the distillate vapor removed from the top of the purification column typically rises above 80% by weight.

In another operation of the purification column 25, the crude alcohol is fed below the top of the column and the dilution water is fed to the top of the column. A purified ethanol-water mixture, typically at a concentration of 8-20% by weight, is removed from the bottom of the column. Unwanted compounds are removed from the top of the purification column as distillate vapor, which is typically less than 30% by weight relative to ethanol. In this mode of operation, the ethanol-containing steam removed from the top of the purification column does not need to be returned to the top of the column after condensation because the dilution water fed to the top of the column acts as a reflux stream at the top of the column.

In both purification column modes, the column is boiled with steam by passing it either directly to the bottom of the column or indirectly with steam through a heat-5 exchanger. In both modes of operation, the external energy requirement of the purification column is typically 1-3 MJ / 1 kg of purified ethanol (100%).

The object of the invention is to provide a method and an apparatus for carrying out purification distillation in such a way that the energy requirement for the distillation is substantially lower than in previously known methods and apparatus.

According to the invention, the energy demand of the purification column is solved in a new and surprising way. With the arrangement according to the invention, the heat content of the steam from the top of the purification column can be used directly for boiling the bottom space of the same column. According to the invention, the steam from the top of the purification column does not need to be compressed mechanically or by other means to raise its temperature.

In the case of a two-component liquid mixture, the mixture to be purified or another component, e.g. a component boiling at a lower temperature, is fed to the purification column several bottoms below the top bottom of the column 25. To λ .; ta component, es .on.

the higher boiling diluent is passed to the purification column above the lower boiling component feed point and / or to the top of the column. The diluent feed and operating conditions of the 30 columns are adjusted as shown below so that the top temperature of the column is higher than the bottom temperature of the column. In this case, the steam from the top of the column can be used to boil the bottom space of the column.

The apparatus according to the invention comprises means for supplying a diluent to the upper bottom below it or to both the upper bottom and its

II

5 80218 below. The apparatus further includes means for supplying the liquid mixture to be cleaned below the dilution liquid supply point. What is new in the apparatus according to the invention are devices for conducting the heat content of the distillate steam from the top of the column partly to the bottom space of the column, e.g. by means of a heat exchanger connected to boil the bottom space of the column.

In practice, it was found that the temperature of the distillate vapor removed from the top of the purification-10 column included in the potable alcohol purification distillation system is higher than the boiling point of the bottom. Upon closer examination, it was found that the temperatures of the distillate vapor removed from the top of the purification column and the bottom boiling liquid varied greatly depending on the operating conditions of the column. In the first purification column operation, the boiling temperature of the bottom was always clearly higher than the temperature of the distillate vapor removed from the top of the column because the ethanol content of the bottom was lower and the pressure higher than the distillate vapor removed from the top. In another purification column operation, the amount of dilution water, the location of the crude alcohol feed point in the column, and the boiling rate of the column can strongly influence the temperature of the distillate vapor removed from the top of the column and to a lesser extent the boiling point of the column bottom. When the dilution water is fed to the top of the column, it causes a decrease in the ethanol content of the liquid boiling at the bottom of the top of the column, resulting in an increase in the temperature of the distillate vapor removed from the top. If the amount of dilute water is large enough, the temperature of the distillate vapor removed from the top of the column will rise higher than the boiling point of the liquid boiling in the bottom space of the column. This temperature difference is larger the smaller the pressure drop of the purification column, i.e. the pressure difference between the bottom and the 35 peaks.

Typically, 25 to 50 bell, screen or valve bases are used in the purification column, with which the pressure drop of the column in the distillation situation is typically 75 to 250 mbar. When using low pressure loss packed column packings, the column pressure difference can be kept below 50 mbar.

By adjusting the distillation conditions of the purification column so that the temperature of the distillate vapor removed from the purification column is higher than the boiling point of the bottom, it is possible to transfer the energy of the distillate vapor through a heat exchanger to boil

In the process according to the invention, the distillate steam leaving the top of the purification column is passed essentially as such and directly from the top to the secondary side of a heat exchanger connected to the bottom space of the same column, so that the distillate steam condenses partially or completely. in the converter, giving up its condensing energy to boil the column.

With the arrangement according to the invention, the need for external energy of the purification column can be substantially reduced.

The apparatus solution according to the invention can also be used in other ways than for the purification distillation of crude alcohol or impure alcohol produced by fermentation, such as alcohol produced by a synthetic route.

When using the method according to the invention for the purification of alcohol, the concentration of the alcohol to be purified is e.g. 20 to 90% by weight. Typically, the alcohol to be purified is the crude alcohol leaving the mash column, concentration 30-50% by weight. In another typical case, the alcohol to be purified is a crude alcohol having a concentration of, for example, 88 to 94% by weight.

The process and distillation apparatus of the invention are also suitable for the purification of liquid pairs other than water-ethanol mixtures. In this case, for example, liquid pairs formed by water and other alcohols,

II

7 80218 Liquid pairs of water and other organic liquids and / or liquid pairs of organic liquids in general.

The invention will now be described in detail by way of example with reference to the accompanying drawings, in which Figure 1 shows an industrial scale, prior art apparatus as a flow chart, and Figure 2 shows a method and apparatus according to the invention as a flow chart.

Example 1:

In one distillery, the purification column shown in Figure 1 was used. The column was a 42-bottom 15 bell-bottom column.

Crude alcohol, such as distillate from the mash column, was fed along feed line 2 to the middle stages of purification column 1. The raw alcohol feed may be preheated in one of the other 20 heat exchangers in the distillation system.

Sufficient dilution water, preferably close to the top temperature of the column, e.g. from the bottom space of the concentration column in the distillation system, is fed to the top 25 buoys of the purification column along feed line 1.

A dilute purified alcohol solution, typically containing 8-20% by weight of ethanol, was passed from the bottom space 6 of the purification column along the discharge line 7 for further processing elsewhere in the distillation system.

The ethanol-containing steam leaving the top 5 of the purification column 5 is led to the heat exchanger 12 to be condensed in line 4. The condensed steam, the so-called the distillate was removed from the heat exchanger along line 10 and passed on for further processing elsewhere in the distillation system.

35 In addition, the apparatus included a heat exchanger 8 connected to the bottom space of the column. Primary steam was supplied to the primary side of the heat exchanger along line 10.

8 80218

Condensed steam, so-called the primary condensate was removed from the heat exchanger along the discharge line 11 and passed on for further processing elsewhere in the distillation system. The thermal energy 5 released during the condensation of the primary steam was transferred to the secondary side of the heat exchanger and from there along line 9 to the bottom space of the purification column, causing the liquid in the bottom space of the purification column to boil.

At the alcohol plant, the material and energy balance shown in Table 1 was measured for the 10 purification columns shown in Fig. 1.

From the material balance, it was found that the temperature of the ethanol-containing steam (stream 4) leaving the top of the purification column was in practice 15 higher than the boiling point of the same column bottom (flow 7), and ethanol-injected steam can be used to boil the bottom of the same column.

20 11 9 80218

Table 1: Material and energy balance flow in and out ent.

EtOH tot. EtOH tot. +/- 5 kg / h kg / h kg / h kg / h MJ / h 2. Raw alcohol feed 1556 2961 + 589

1288 mbar, 60 ° C

10 3. Dilution water - 0 11000 + 4795 supply

1204 mbar, 104 ° C

4. Distillate steam, 29 1098 -2909

1204 mbar, 105 ° C

7. Base product, 1527 12863 -5102

1364 mbar, 99.1 ° C

20 10. steam 0 1193 +3228

2 bar, 120 ° C

11. primary condensate 0 1193 -601

2 bar, 120 ° C

25 _ column sum 1556 15154 1556 15154 0 abbreviations:

EtOH = mass flow of ethanol 30 tot. = total ssavir flow ent = flow enthalpy; liquid at 0 ° C enthalpy calculation reference level + = direction of enthalpy flow from outside to inside the balance limit 35 - = direction of enthalpy flow from inside the balance limit outwards 10 80218

Example 2.

From the material and energy balance shown in Table 1, the heat input to heat exchanger 8 in Example 1 can be calculated as follows: 5 + 32238 MJ / h to 601 MJ / h 2627 MJ / h (flow 10) (flow 11) 10 It can be calculated that the distillate steam flow of Example 1 4 condenses at a pressure of 1204 mbar as follows: 1098 kg / h -----> 1098 kg / h + 2427 MJ / h 15 distillate steam condensate heat of condensation

1204 mbar, 105 ° C 1204 mbar, 101.9 ° C

Since the distillate steam stream 4 contains 2.64 wt% ethanol, the temperature drops from 105 ° C to 101.9 ° C during total condensation. Since the condensing temperature of the total condensing is higher than the bottom temperature of the purification column in Example 1, the distillate steam can be directed to the boiling heat exchanger of the purification column as shown in Fig. 2 and 23 the entire condensing heat can be transferred to boiling the purification column.

In order to maintain the thermal balance of the column, the primary boiling energy must also be fed to the column as shown in Figure 2, heat exchanger 8b, the following amount: 2627 MJ / h -2427 MJ / h = 200 MJ / h boiling power of the condensing heat of the steam flow (4)

Example 2 shows that according to the invention

II

11 8021 8 the need for external boiling energy is reduced from 2627 MJ / h to 200 MJ / h.

The embodiments are intended only to illustrate the invention, and embodiments of the invention may vary within the scope of the appended claims.

Claims (10)

    12 8021 8
  1. A method for purifying a two-component liquid mixture of impurities by distillation, wherein the liquid mixture to be purified is fed to a purification column between the bottom space and the top, the second component of the liquid mixture is fed to the column as a diluent, - that the heat content of the distillate to be removed from the top of the column is at least partially conducted to the bottom space of the column, e.g. by passing the distillate to a heat exchanger arranged to heat the bottom space.
  2. Process according to Claim 1, characterized in that the temperature of the distillate to be removed from the top of the column is higher than the temperature of the bottom of the column.
  3. Process according to Claim 1 or 2, characterized in that the second component of the two-component liquid mixture is introduced into the column as a diluent above the feed point of the liquid mixture to be purified.
  4. Process according to one of Claims 1 to 3, characterized in that the second component of the two-component liquid mixture is introduced into the column as a diluent at the top of the column.
  5. Process according to one of Claims 1 to 4, characterized in that the liquid mixture to be purified is an ethanol-water mixture.
  6. Process according to Claim 5, characterized in that the ethanol-water mixture contains 20 to 95% by weight of ethanol.
  7. Process according to Claims 3 and 4, characterized in that the concentration of steam leaving the top of the column is less than 30% by weight of ethanol.
  8. 8. Distillation apparatus for purifying a two-component liquid mixture from impurities by distillation, the apparatus comprising a multi-bottomed purification column (1); feeding devices (2) for feeding the mixture to be cleaned below the top bottom; supply means (3) for passing the second component of the liquid mixture to the purification column as a diluent; peak removal (4), to remove distillate vapors from the top of the column (5); removing the bottom (6) (7) to remove the bottom product from the bottom of the column; characterized in that the apparatus comprises 10 heat exchangers (8), the peak removal, i.e. the distillate vapors are passed from the top (5) of the column to a heat exchanger (8) arranged to conduct the heat content of the distillate vapors at least in part to the bottom space of the column (1).
  9. Method according to claim 8, characterized in that the diluent supply device (3) is arranged to supply the diluent to the top bottom of the column and the liquid mixture feed devices (2) are arranged to supply the liquid mixture below the top bottom of the column.
  10. Apparatus according to claim 8, characterized in that the apparatus comprises a heat exchanger (8b) by means of which the thermal power required to start the column and the thermal power required to maintain the energy balance of the column are fed to the bottom of the purification column (1). ! 4 80218
FI886052A 1988-12-30 1988-12-30 Process and plant for purification of a two-component liquid mixture by distillation FI80218C (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
FI886052A FI80218C (en) 1988-12-30 1988-12-30 Process and plant for purification of a two-component liquid mixture by distillation
FI886052 1988-12-30

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
FI886052A FI80218C (en) 1988-12-30 1988-12-30 Process and plant for purification of a two-component liquid mixture by distillation
PCT/FI1990/000002 WO1990007367A1 (en) 1988-12-30 1990-01-02 Method and apparatus for the purification of a two-component liquid mixture by distillation
EP19900901597 EP0456647A1 (en) 1988-12-30 1990-01-02 Method and apparatus for the purification of a two-component liquid mixture by distillation
AU48223/90A AU4822390A (en) 1988-12-30 1990-01-02 Method and apparatus for the purification of a two-component liquid mixture by distillation

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FI80218B FI80218B (en) 1990-01-31
FI80218C true FI80218C (en) 1990-05-10

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AU (1) AU4822390A (en)
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WO (1) WO1990007367A1 (en)

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FI80218B (en) 1990-01-31
WO1990007367A1 (en) 1990-07-12
EP0456647A1 (en) 1991-11-21
AU4822390A (en) 1990-08-01

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