RU2480445C2 - Method of separating liquid phase by-products of fischer-tropsch synthesis - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of separating liquid phase by-products of Fischer-Tropsch synthesis, which involves the following steps: a) feeding the liquid phase by-products into a standard fractionation column (1) in its middle part with output of a portion of the stream I, having a boiling point range from 50 to 120°C, as a side cut to obtain light components having boiling point below 50°C from the top of the column, and heavy components, having boiling point higher than 120°C from the bottom of the column; b) feeding the stream I into a column (2) for separating acetic acid in its middle part to obtain a stream of aqueous solution II, containing alcohols and ketones, having boiling point range from 50 to 100°C from the top of the column, and a stream III of aqueous solution of acetic acid from the bottom of the column; and c) feeding the stream II into a column (3) for separating ethanol in its middle part to obtain a stream IV of a mixture of methanol and acetone from the top of the column and a stream V of aqueous solution of ethanol and n-propanol from the bottom of the column (see dwg 3).

EFFECT: high efficiency of the process.

9 cl, 4 dwg, 30 tbl, 30 ex

Description

Cross reference to related applications

This application claims priority on the basis of applications No. CN 200810032926.3 of January 23, 2008, CN 200810032927.8 of January 23, 2008, CN 200810043253.1 of April 11, 2008 and CN 200810043252.7 of April 11, 2008, which are given here for information.

FIELD OF THE INVENTION

The present invention relates to a method for separating by-products in the aqueous phase of the Fischer-Tropsch synthesis.

State of the art

As demand for petroleum-based liquid fuels increases and available stocks of oil sources decrease, methods for producing used liquid fuels from solid fuels such as coal are attracting increasing attention. A method of producing liquid fuels from solid fuels, well known to those skilled in the art, is the so-called Fischer-Tropsch synthesis process, in which synthesis gas, including carbon monoxide and hydrogen, is obtained from a carbon material such as coal in the presence of a catalyst based on iron, a catalyst based on cobalt or a catalyst based on iron and cobalt, at a certain temperature and a certain pressure is catalytically converted to methane and hydrocarbons, having a greater number of carbon atoms, with the simultaneous formation of alcohols, other oxygen-containing compounds, water and the like.

The water in the Fischer-Tropsch synthesis reaction product stream can be easily separated from hydrocarbons as the main Fischer-Tropsch synthesis product, but the water recovered from the Fischer-Tropsch synthesis reaction product stream will contain some organic oxygen-containing compounds such as alcohols, aldehydes , ketones, acids, and the like due to the solubility of these organic oxygenated compounds in water.

Since the amount of water generated during the Fischer-Tropsch synthesis process is relatively large, the direct discharge of water is obviously wasteful and does not comply with environmental regulations due to the presence of organic oxygen-containing compounds such as alcohols, aldehydes, ketones, acids and the like, which can cause corrosion and pollution. Patent application CN 1696082A simply discloses a method for separating by-products of the Fischer-Tropsch synthesis in the aqueous phase, in which the by-products in the aqueous phase are separated by standard distillation to form a mixture of light oxygen-containing compounds such as alcohols and ketones containing a small amount of water and water-containing oxygen compounds having higher boiling points, using as a fuel a mixture obtained from the top of the distillation column, and water from the bottom of the column is drawn into recycling back to the synthesis gas production step to form a suspension with solid components such as coal. The method disclosed in the aforementioned patent application does not provide sufficient use of basic organic materials contained in by-products in the aqueous phase.

Therefore, there is still a need for a method for separating the by-products of the Fischer-Tropsch synthesis in the aqueous phase, by which the by-products of the Fischer-Tropsch synthesis in the aqueous phase can be utilized sufficiently and problems associated with environmental pollution can be solved.

SUMMARY OF THE INVENTION

The problem to which the present invention is directed, is to provide a method of separating the by-products of the Fischer-Tropsch synthesis in the aqueous phase, including stages

a) feeding the by-products in the aqueous phase to a standard distillation column (1) in its middle part with the withdrawal of part of stream I having a boiling point in the range from 50 to 120 ° C as a side stream, to obtain light components having a boiling point of less than 50 ° C, from the top of the column, and to obtain heavy components having boiling points higher than 120 ° C, from the bottom of the column;

b) supplying stream I to the column (2) for separating acetic acid in its middle part to obtain stream II of an aqueous solution containing alcohols and ketones having a boiling range of 50 to 100 ° C from the top of the column and to obtain stream III of an aqueous solution of acetic acids from the bottom of the column; and

c) feeding stream II to the ethanol separation column (3) in its middle part, to obtain stream IV of a mixture of methanol and acetone from the top of the column, and to obtain stream V of an aqueous solution of ethanol and n-propanol from the bottom of the column.

Another objective of the present invention is to provide a method for the separation of by-products of the Fischer-Tropsch synthesis in the aqueous phase, which includes stages

a) feeding the by-products in the aqueous phase to a standard distillation column (201) in its middle part, with the withdrawal of part of stream I having a boiling range of 50 to 120 ° C as a side stream, to obtain light components having a boiling point of less than 50ºС, from the top of the column, and with obtaining heavy components having boiling points higher than 120ºС, from the bottom of the column;

b) supplying stream I to one side of the section column (202) in its middle part, removing stream II of a methanol / acetone mixture as a distillate from the top of the column, removing stream III of an aqueous solution of acetic acid from the bottom of the column, removing ethanol as side stream from the upper part of the opposite side and with the withdrawal of stream IV of an aqueous solution of n-propanol as a side stream from the lower part of the opposite side.

Brief Description of the Drawings

Figure 1 is a schematic graphical representation of a process for separating by-products of a Fischer-Tropsch synthesis in an aqueous phase according to an embodiment of the process of the first aspect of the invention.

Figure 2 is a schematic diagram of a process for separating by-products of the Fischer-Tropsch synthesis in the aqueous phase according to a preferred embodiment of the process of the first aspect of the invention.

Figure 3 is a schematic diagram of a process for separating by-products of the Fischer-Tropsch synthesis in the aqueous phase according to an embodiment of the process of the second aspect of the invention.

Figure 4 is a schematic diagram of a process for separating by-products of Fischer-Tropsch synthesis in the aqueous phase according to a preferred embodiment of the process of the second aspect of the invention.

Detailed Description of Preferred Embodiments

In a first embodiment, the present invention provides a method for separating by-products of Fischer-Tropsch synthesis in an aqueous phase (hereinafter referred to as the process of the first aspect of the invention), comprising the steps of

a) feeding the by-products in the aqueous phase to a standard distillation column (1) in its middle part with the removal of part of stream I having a boiling range of 50 to 120 ° C as a side stream, to obtain light components having a boiling point of less than 50 ° C , from the top of the column, and to obtain heavy components having boiling points higher than 120 ° C, from the bottom of the column;

b) supplying stream I to the column (2) for separating acetic acid in its middle part, to obtain stream II of an aqueous solution containing alcohols and ketones having a boiling range of 50 to 100 ° C from the top of the column, and to obtain stream III of an aqueous solution acetic acid from the bottom of the column; and

c) feeding stream II to the ethanol separation column (3) in its middle part to obtain stream IV of a mixture of methanol and acetone from the top of the column and to obtain stream V of an aqueous solution of ethanol and n-propanol from the bottom of the column.

In this process, a standard distillation column 1 may have a number of theoretical plates from 10 to 60, a reflux ratio from 1 to 12, a top temperature of the column of at least 40 ° C and a side temperature of 80 to 90 ° C; the acetic acid separation column 2 may have a number of theoretical plates from 10 to 50, a reflux number from 1 to 8, and a bottom temperature of the column from 104 to 108 ° C; and the ethanol separation column 3 may have a theoretical plate number of from 20 to 80, a reflux ratio of 2 to 10, and a column top temperature of 60 to 64 ° C.

In a preferred embodiment, the process of the first aspect according to the invention further comprises the steps of

d) supplying stream III to the top of the acetic acid extraction column 4 to obtain a stream VIII of an acetic acid / extraction reagent mixture from the top of the column and to produce wastewater from the bottom of the column in which the extracting reagent is at least one reagent selected from the group consisting of organic phosphines and organic amines; and

f) supplying stream VIII to the column 5 for regeneration of the extracting reagent in its middle part with removal of acetic acid as a distillate from the top of the column and obtaining a regenerated extracting reagent from the bottom of the column.

Acetic acid extraction column 4 may have a number of theoretical plates of 10 to 40 and may operate at normal temperature. The extraction reagent applicable in acetic acid extraction column 4 is preferably at least one reagent selected from the group consisting of three (C1-C6-alkyl) phosphinoxides, triphenylphosphine oxide, tert-butylamine, n-butylamine and tert-amylamine, and the weight ratio of extracting reagent to stream III can be from 1 to 6. Column 5 of regeneration of extracting reagent can have a number of theoretical plates from 10 to 50 and reflux ratio from 1 to 6. Column 5 of regeneration of extracting reagent can work at atmospheric pressure or reduced pressure, and preferably under reduced pressure, and the top temperature of the column can be adjusted to a level near the boiling point of acetic acid at a working pressure, preferably in the range of said boiling point ± 1.0 ° C.

In a preferred embodiment, the process of the first aspect of the invention further comprises the steps of

f) feeding stream IV to extractive distillation column 6 in its middle part and supplying a polar solvent to extractive distillation column 6 above its middle part, removing acetone from the top of the column and stream VI of methanol / solvent mixture from the bottom of the column; and

g) feeding stream VI to the column 7 of solvent regeneration in its middle part with the removal of methanol from the top of the column and obtaining a regenerated solvent from the bottom of the column

Extractive distillation column 6 may have a number of theoretical plates from 20 to 50, a reflux number from 2 to 9, and a column top temperature from 56 to 56.5 ° C. In extractive distillation column 6, the weight ratio of polar solvent to stream IV may range from 2 to 10. Examples of polar solvents include, but are not limited to, water, ethylene glycol, N-formyl morpholine, tetramethylene sulfone, and monoethanolamine. The solvent regeneration column 7 may have a number of theoretical plates from 10 to 50, a reflux number from 1 to 6, and a column top temperature from 64.5 to 64.7 ° C.

In a preferred embodiment, the process of the first aspect of the invention further comprises the steps of

h) feeding stream V to column 8 of ethanol removal in its middle part, removing ethanol from the top of the column and obtaining stream VII of an aqueous solution of n-propanol from the bottom of the column; and

i) feeding stream VII to azeotropic distillation column 9 in its middle part, and jointly supplying the azeotropically forming agent, with the removal of the aqueous phase obtained in the phase separator at the top of the column, with reflux by reflux from the oil phase obtained in the phase separator, and with the removal of n-propanol from the bottom of the column, in which the azeotropic agent is at least one agent that forms an azeotropic mixture with water at a lower boiling point.

The ethanol removal column 8 may have a number of theoretical plates from 10 to 60, a reflux number from 1 to 8, and a top temperature of the column from 68 to 68.5 ° C. Column 9 of azeotropic rectification may have a number of theoretical plates from 15 to 60, the weight ratio of the azeotropic agent to flow VII from 0.2 to 1, and the bottom temperature of the column from 96.8 to 97.5 ° C. Examples of azeotropically forming agents include, but are not limited to, cyclohexane, benzene, toluene, isopropyl acetate and n-butyl acetate.

Since the by-products in the aqueous phase of the Fischer-Tropsch synthesis are complex, the standard distillation process can be used first to remove a small amount of lighter components and a small amount of heavier components and to remove the main amount of medium components as a side stream. More than 80 weight percent of the side stream may be water. To reduce energy consumption, the bulk of the water is removed as a heavy component from the bottom of the acetic acid separation column. The extraction process can be used to separate acetic acid from water in an aqueous solution of acetic acid obtained from the bottom of the acetic acid separation column. The components obtained from the top of the acetic acid separation column can be separated in the ethanol separation column 3 by conventional distillation into an acetone / methanol mixture stream and an ethanol / n-propanol aqueous solution stream. By the process of the first aspect of the invention, good separation of by-products in the aqueous phase of the Fischer-Tropsch synthesis is possible and a good technical effect is achieved.

A specific embodiment of the method according to the first embodiment of the invention will be described in detail below with reference to Figure 1.

In Figure 1, code number 1 indicates a standard distillation column, 2 represents an acetic acid separation column, 3 represents an ethanol separation column, 4 represents an extraction column, 5 represents an extraction reagent recovery column, 10 represents a by-product stream in the aqueous phase, 11 represents a stream of light components 12 represents a stream of heavy components, 13 represents a stream of side stream, 14 represents a stream of an aqueous solution containing alcohols and ketones, 15 represents a stream of aq. solution of acetic acid, 16 represents a stream of extraction reagent, 17 represents a stream of a mixture of methanol / acetone, 18 represents a stream of an aqueous solution of ethanol / n-propanol, 19 represents a stream of a mixture of acetic acid / extracting reagent, 20 represents a stream of acetic acid, 21 represents a stream of regenerated extraction reagent, 22 represents a wastewater stream.

As shown in Figure 1, stream 10, consisting of by-products in the aqueous phase, is fed to a standard distillation column 1 in its middle part, to obtain a stream of 11 light components as distillate from the top of the column, to obtain a stream of 12 heavy components from the bottom of the column and a stream 13 output as side stream. The side stream 13 is fed to the column 2 for separating acetic acid in its middle part to obtain a stream 14 of an aqueous solution containing alcohols and ketones as a distillate from the top of the column and to obtain a stream 15 of an aqueous solution of acetic acid from the bottom of the column. A stream of solution 14, containing alcohols and ketones, is fed to the ethanol separation column 3 in its middle part to obtain a stream of acetone / methanol mixture 17 as a distillate from the top of the column and to obtain a stream of 18 aqueous solution of ethanol and n-propanol from the bottom of the column. Stream 15 of an aqueous solution of acetic acid and stream 16 of extraction reagent are fed to the top and bottom of extraction column 4, respectively, to obtain stream 19 of a mixture of acetic acid and extraction reagent from the top of the column and stream 22 of wastewater discharged from the bottom of the column.

Figure 2 depicts another specific embodiment of the process of the first embodiment of the invention. In Figure 2, code number 1 indicates a standard distillation column, 2 represents an acetic acid separation column, 3 represents an ethanol separation column, 4 represents an extraction column, 5 represents an extraction reagent recovery column, 6 represents an extractive distillation column, 7 represents a solvent regeneration column, 8 represents an ethanol removal column, 9 represents an azeotropic distillation column, 10 represents a stream consisting of by-products in the aqueous phase, 11 represents there is a stream of light components, 12 represents a stream of heavy components, 13 represents a stream of side stream, 14 represents a stream of an aqueous solution containing alcohols and ketones, 15 represents a stream of an aqueous solution of acetic acid, 16 represents a stream of an extraction reagent, 17 represents a stream of a mixture of methanol / acetone, 18 represents a stream of an aqueous solution of ethanol and n-propanol, 19 represents a stream of a mixture of acetic acid / extraction reagent, 20 represents a stream of acetic acid, 21 represents a stream of regenerated a reagent, 22 represents a waste water stream, 23 represents a solvent stream, 24 represents an acetone stream, 25 represents a methanol / solvent mixture stream, 26 represents an ethanol stream (95 weight percent), 27 represents an n-propanol aqueous solution stream, 28 represents a methanol stream , 29 represents a stream of regenerated solvent, 30 represents an azeotropic aqueous stream, and 31 represents a stream of n-propanol.

As shown in Figure 2, stream 10, consisting of by-products in the aqueous phase, is supplied to a standard distillation column 1 to obtain a stream of 11 light components as distillate from the top of the column, to obtain a stream of 12 heavy components from the bottom of the column and stream 13 obtained as a side shoulder strap. A side stream stream 13 is fed to the acetic acid separation column 2 to obtain an aqueous solution stream 14 containing alcohols and ketones as a distillate from the top of the column, and to obtain an aqueous acetic acid stream 15 from the bottom of the column. Stream 14 is fed to ethanol separation column 3 to obtain acetone / methanol mixture stream 17 as a distillate from the top of the column and to obtain stream 18 of an n-propanol aqueous solution from the bottom of the column. Stream 15 of an aqueous solution of acetic acid and stream 16 of extraction reagent are fed into extraction column 4 to its top and bottom, respectively, to obtain stream 19 of a mixture of acetic acid / extraction reagent from the top of the column and to obtain a stream 22 of wastewater from the bottom of the column. The methanol / acetone mixture stream 17 and the solvent stream 23 are fed to the extractive distillation column 6 in its middle part and the middle of the upper part, respectively, to obtain acetone stream 24 as distillate from the top of the column and to obtain methanol / solvent mixture stream 25 from the bottom of the column . Stream 18 of an aqueous solution of ethanol and n-propanol is supplied to the ethanol removal column 8 to obtain a stream of 26 ethanol (95 weight percent) as a distillate from the top of the column and to obtain a stream 27 of an aqueous solution of n-propanol from the bottom of the column. Acetic acid / extraction reagent mixture stream 19 is supplied to the extraction reagent recovery column 5 to obtain acetic acid stream 20 as a distillate from the top of the column and to obtain a regenerated extraction reagent stream 21 from the bottom of the column. The methanol / solvent mixture stream 25 is supplied to the solvent regeneration column 7 to obtain a methanol stream 28 as a distillate from the top of the column and to obtain a regenerated solvent stream 29 from the bottom of the column. Stream 27 of an aqueous solution of n-propanol is supplied to the azeotropic distillation column 9 with the removal of azeotropic water 30 from the top of the column and obtaining a stream of 31 n-propanol from the bottom of the column.

According to a second embodiment, the present invention provides a process for separating by-products in the aqueous phase of the Fischer-Tropsch synthesis (hereinafter referred to as the process of the second aspect of the invention), comprising the steps of

a) feeding the by-products in the aqueous phase to a standard distillation column 201 in its middle part with the withdrawal of a portion of stream I having a boiling range of 50 to 120 ° C as a side stream with light components having a boiling point of less than 50 ° C from the top columns and with obtaining heavy components having boiling points higher than 120 ° C from the bottom of the column;

b) supplying stream I to one side of the section column 202 in its middle part with removal of stream II of a methanol / acetone mixture as a distillate from the top of the column, removing stream III of an aqueous solution of acetic acid from the bottom of the column, with the removal of ethanol as a side stream from the top part of the opposite side and with the removal of stream IV of an aqueous solution of n-propanol as a side stream from the bottom of the opposite side.

Standard distillation column 201 may have a number of theoretical plates from 10 to 60, reflux number from 1 to 12, the temperature of the top of the column is not less than 40 ° C. Sectional column 202 may have a number of theoretical plates from 50 to 200, in which 1/6 to 1/3 of the number of theoretical plates may fall on the upper section, and 1/6 to 1/3 of the number of theoretical plates may fall on the lower section. The liquid phase of the left side in the upper section may have a distribution coefficient from 0.3 to 0.7, and the gas phase of the left side in the lower section may have a distribution coefficient from 0.3 to 0.7. Sectional column 202 may have a reflux number from 5 to 30, a column top temperature from 60 to 64 ° C, an upper sidestream temperature from 68 to 68.5 ° C, and a lower sidestream temperature from 87 to 93 ° C.

In a preferred embodiment, the process of the second aspect of the invention further comprises the steps of

c) feeding stream IV to the azeotropic distillation column 203 in its middle part and jointly bringing the azeotropically forming agent to it, removing the aqueous phase obtained in the phase separator of the top of the column and refluxing from the oil phase, and removing n-propanol from the bottom of the column, wherein the azeotropically forming agent is at least one agent that forms an azeotropic mixture with water with a lower boiling point.

The azeotropic distillation column 203 may have a number of theoretical plates from 15 to 60, the weight ratio of the azeotropic agent to stream IV from 0.2 to 1, and the bottom temperature of the column from 96.8 to 97.5 ° C. The azeotropically forming agent is preferably a single substance from cyclohexane, benzene, toluene, isopropyl acetate and n-butyl acetate.

In a preferred embodiment, the method according to the second embodiment of the invention further comprises the steps of

d) supplying stream III to the top of the acetic acid extraction column and extraction reagent 204 to the bottom of the column, discharging stream V of the mixture of acetic acid and extraction reagent from the top of the column and discharging waste water from the bottom of the column in which the extraction reagent is at least one a reagent selected from the group consisting of organic phosphines and organic amines; and

f) feeding stream V to the recovery agent regeneration column 205 in its middle portion, removing acetic acid as a distillate from the top of the column and obtaining a regenerated extracting agent from the bottom of the column.

Acetic acid extraction column 204 may have a number of theoretical plates from 10 to 40 and a weight ratio of extracting reagent to stream III from 1 to 6 and may operate at normal temperature. The extraction reagent regeneration column 205 may have a number of theoretical plates from 10 to 50 and the reflux ratio from 1 to 6. The extracting reagent regeneration column 205 may operate at atmospheric pressure or under reduced pressure, and preferably under reduced pressure. The applicable extracting reagent is preferably at least one reagent selected from the group consisting of three (C1-C6-alkyl) phosphine oxides, triphenylphosphine oxide, tert-butylamine, n-butylamine and tert-amylamine.

In a preferred embodiment, the method according to the second embodiment of the invention further comprises the steps of

f) feeding stream II to extractive distillation column 206 in its middle portion and a polar solvent to its upper section, removing acetone as a distillate from the top of the column and stream VI of a mixture of methanol and solvent from the bottom of the column; and

g) feeding stream VI to the solvent regeneration column 207 in its middle portion, removing methanol as a distillate from the top of the column and obtaining a regenerated solvent from the bottom of the column.

The extractive distillation column 206 may have a number of theoretical plates from 20 to 50, a weight ratio of polar solvent to stream VI from 2 to 10, a reflux ratio from 2 to 9, and a column top temperature from 56 to 56.5 ° C. The polar solvent is preferably at least one solvent of water, ethylene glycol, N-formylmorpholine, tetramethylene sulfone and monoethanolamine. The solvent regeneration column 207 may have a number of theoretical plates from 10 to 50, a reflux number from 1 to 6, and a column top temperature from 64.5 to 64.7 ° C.

Since the by-products in the aqueous phase of the Fischer-Tropsch synthesis are complex, the standard distillation method can be used first to remove a small amount of lighter components and a small amount of heavier components and to remove the main amount of medium components as a side stream. More than 80 weight percent of the side stream may be water. To reduce energy consumption, the main amount of water is removed as a heavy component from the bottom of the section column, the acetone / methanol mixture is obtained from the top of the column, ethanol is discharged as an upper side stream, and an aqueous solution of n-propanol is discharged as a lower side stream. The extraction process can be used to separate acetic acid from water in an aqueous solution of acetic acid obtained from the bottom of a section column. An aqueous solution of n-propanol is separated using the azeotropic fractionation process. By the process of the second aspect of the invention, good separation of by-products in the aqueous phase of the Fischer-Tropsch synthesis is possible and a good technical effect is achieved.

A specific embodiment of the method according to the second embodiment of the invention will be described in detail below with reference to Figure 3.

In Figure 3, code number 201 denotes a standard distillation column, 202 represents a section column, 203 represents an azeotropic distillation column, 204 represents an acetic acid extraction column, 205 represents an extraction reagent recovery column, 208 represents a by-product stream in the aqueous phase of the Fischer synthesis Tropsch, 209 represents a stream of light components, 210 represents a stream of heavy components, 211 represents a stream of side stream, 212 represents a stream of a mixture of methanol / acetone, 2 13 represents an ethanol stream, 214 represents an aqueous solution of n-propanol, 215 represents an aqueous solution of acetic acid, 216 represents an extracting reagent stream, 217 represents an azeotropic water stream, 218 represents an n-propanol stream, 219 represents an acetic acid / extracting mixture stream , 220 represents a stream of wastewater, 221 represents a stream of acetic acid, and 222 represents a stream of regenerated extraction reagent.

As shown in Figure 3, stream 208, consisting of by-products in the aqueous phase, is fed to a standard distillation column 201 in its middle portion to obtain a stream of 209 light components as distillate from the top of the column, to obtain a stream of 210 heavy components from the bottom of the column and a stream 211 obtained as side stream. Side run 211 is fed to sectional column 202 in its middle part on its left side, to obtain acetone / methanol mixture stream 212 as distillate from the top of the column, to obtain stream 215 of an aqueous solution of acetic acid obtained from the bottom of the column, to obtain ethanol stream 213 as a side stream from the upper part of the right side and to obtain a stream 214 of n-propanol as a side stream from the lower part of the right side. Stream 214 of an aqueous solution of n-propanol is supplied to the azeotropic distillation column 203 in its middle part, with the removal of azeotropic water stream 217 as the aqueous phase of the top of the column and obtaining stream 218 of n-propanol from the bottom of the column. Acetic acid aqueous solution stream 215 and an extraction reagent stream 216 are supplied to an acetic acid extraction column 204 at its upper and lower parts, respectively, to obtain an acetic acid / extraction reagent mixture stream 219 from the top of the column and wastewater stream 220 discharged from the bottom of the column . Acetic acid / extraction reagent mixture stream 219 is supplied to the extraction reagent recovery column 205 in its middle portion to produce acetic acid stream 221 as distillate from the top of the column and to obtain a regenerated extraction reagent stream 222 from the bottom of the column.

In Figure 4, code number 201 denotes a standard distillation column, 202 represents a sectional column, 203 represents an azeotropic distillation column, 204 represents an acetic acid extraction column, 205 represents an extraction reagent recovery column, 206 represents an extractive distillation column, 207 represents a solvent regeneration column, 208 represents a stream consisting of by-products in the aqueous phase, 209 represents a stream of light components, 210 represents a stream of heavy components, 211 p represents a side stream, 212 represents a stream of methanol / acetone mixture, 213 represents a stream of ethanol, 214 represents a stream of an aqueous solution of n-propanol, 215 represents a stream of an aqueous solution of acetic acid, 216 represents a stream of extraction reagent, 217 represents a stream of azeotropic water, 218 represents a stream n-propanol, 219 represents a stream of a mixture of acetic acid / extraction reagent, 220 represents a stream of wastewater, 221 represents a stream of acetic acid, 222 represents a stream of regenerated extracting o reagent, 223 represents a solvent stream, 224 represents an acetone stream, 225 represents a methanol / solvent mixture stream, 226 represents a methanol stream and 227 represents a regenerated solvent stream.

As shown in Figure 4, a stream 208, consisting of by-products in the aqueous phase, is fed to a standard distillation column 201 in its middle portion, to obtain a stream of 209 light components as distillate from the top of the column, to obtain a stream of 210 heavy components from the bottom of the column and a stream 211 output as side stream. A side stream stream 211 is supplied to the section column 202 in its middle part on its left side to obtain an acetone / methanol mixture stream 212 as a distillate from the top of the column, to obtain an acetic acid solution stream 215 from the bottom of the column, to obtain ethanol stream 213 as a side stream from the upper part of the right side of the column and to obtain a stream 214 of an aqueous solution of n-propanol as a side stream from the lower part of the right side. The solvent stream 223 and the acetone / methanol mixture stream 212 are fed to the extractive distillation column 206 at its upper and middle parts, respectively, to obtain acetone stream 224 as a distillate from the top of the column and to obtain methanol / solvent mixture stream 225 from the bottom of the column. Stream 214 of an aqueous solution of n-propanol is supplied to the azeotropic distillation column 203 in its middle part, with the removal of azeotropic water stream 217 as the aqueous phase of the top of the column and obtaining stream 218 of n-propanol from the bottom of the column. Acetic acid aqueous solution stream 215 and an extraction reagent stream 216 are supplied to an acetic acid extraction column 204 at its upper and lower parts, respectively, to obtain an acetic acid / extraction reagent mixture stream 219 from the top of the column and wastewater stream 220 discharged from the bottom of the column . The methanol / solvent mixture stream 225 is fed to the middle portion of the solvent regeneration column 207 to obtain a methanol stream 226 as a distillate from the top of the column and a regenerated solvent stream 227 obtained from the bottom of the column. Acetic acid / extraction reagent mixture stream 219 is supplied to the extraction reagent recovery column 205 in its middle portion to produce acetic acid stream 221 as distillate from the top of the column and to obtain a regenerated extraction reagent stream 222 from the bottom of the column.

Examples

The following examples are provided to further illustrate the invention, but in no way limit the invention.

Example 1

As shown in Figure 1, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1, having the number of theoretical plates 15, at the level of the 7th theoretical plate, with the operation of column 1 at reflux number 12 and the top temperature of the columns 40 ° C. The side stream 13, having a boiling range from 50 to 120 ° C, was withdrawn from the level of the 8th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 15 at the level of the 8th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to the ethanol separation column 3 having a theoretical plate number of 20 at the level of the 9th theoretical plate. The ethanol separation column 3 operated at a reflux value of 10 and a column top temperature of 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. A stream 15 from the bottom of the acetic acid separation column and extraction reagent 16 was fed to the acetic acid extraction column 4, having the number of theoretical plates 10, at its top and bottom, respectively. The extraction reagent was tert-butylamine, and the weight ratio of the extraction reagent to stream 15 was 5. Acetic acid extraction column 4 was operated at 35 ° C, a mixture of 19 acetic acid / extraction reagent was obtained from the top of the acetic acid extraction column, and wastewater 22 was obtained from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was fed into the recovery reagent recovery column 5 having a theoretical number of plates 10 at the level of the 4th theoretical plate. Extraction reagent regeneration column 5 was operated at a reflux value of 6 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 20 as a distillate from the top of the column and to obtain a regenerated extracting reagent 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 1.

Table 1
Analytical data (weight percent) for flows of individual columns

Example 2

As shown in Figure 1, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1, having the number of theoretical plates 60, at the level of the 35th theoretical plate. Column 1 operated at a reflux value of 1 and a column top temperature of 40 ° C. Side run 13, having a boiling point range from 50 to 120 ° C, was taken out from the level of the 40th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 50 at the level of the 30th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. The water stream 14 was fed into the ethanol separation column 3 having a theoretical plate number of 80 at the level of the 50th theoretical plate. The ethanol separation column 3 operated at a reflux value of 2 and a column top temperature of 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. A stream 15 from the bottom of the acetic acid separation column and extraction reagent 16 was fed to the acetic acid extraction column 4, having the number of theoretical plates 40, on its top and bottom, respectively. The extraction reagent was n-butylamine, and the weight ratio of the extraction reagent to stream 15 was 1. The column of extraction of acetic acid was operated at a temperature of 35 ° C, a mixture of 19 acetic acid / extraction reagent was obtained from the top of the column of extraction of acetic acid, and wastewater 22 was obtained from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was fed into the recovery reagent recovery column 5 having the number of theoretical plates 50 at the level of the 20th theoretical plate. Extraction reagent regeneration column 5 was operated at a reflux value of 1 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 20 as a distillate from the top of the column and to obtain a regenerated extracting reagent 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 2.

table 2
Analytical data (weight percent) for flows of individual columns

Example 3

As shown in Figure 1, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling point of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1, having the number of theoretical plates 30, at the level of the 17th theoretical plate. Column 1 operated at a reflux value of 3 and a column top temperature of 1 ° C. The side stream 13, having a boiling range of 50 to 120 ° C, was taken out from the level of the 20th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 30 at the level of the 17th theoretical plate. Column 2 operated at a reflux value of 4 and a bottom temperature of the column from 104 to 108 ° C to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to ethanol separation column 3 having a theoretical plate number of 40 at the level of the 25th theoretical plate. Column 3 operated at a reflux value of 4 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream of 18 aqueous solution of ethanol and n-propanol from the bottom of the column. A stream 15 from the bottom of the acetic acid separation column and extraction reagent 16 was fed to the acetic acid extraction column 4, having the number of theoretical plates 20, on its top and bottom, respectively. The extraction reagent was trimethylphosphine oxide, and the weight ratio of the extracting reagent to stream 15 was 2. Column 4 was operated at a temperature of 35 ° C, a mixture of 19 acetic acid / extracting reagent was obtained from the top of the column and wastewater 22 was obtained from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was fed into the recovery reagent recovery column 5 having a theoretical plate number of 25 at the level of the 10th theoretical plate. Column 5 was operated at a reflux value of 3 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 20 as a distillate from the top of the column and to obtain a regenerated extractant 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 3.

Table 3
Analytical data (weight percent) for flows of individual columns

Example 4

The procedure was followed as described in Example 3, except that triphenylphosphine oxide was used as the extraction reagent in the acetic acid extraction column 4. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 4.

Table 4
Analytical data (weight percent) for flows of individual columns

Example 5

The procedure was followed as described in Example 3, except that the by-products in the aqueous phase of the Fischer-Tropsch synthesis had the composition: 7 weight percent of a component having a boiling point of less than 50 ° C., 84 weight percent of a component having a boiling range of 50 to 120 ° C, and 9 weight percent of a component having a boiling point of more than 120 ° C. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 5.

Table 5
Analytical data (weight percent) for flows of individual columns

Example 6

As shown in Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1 having a number of theoretical plates of 15, at the level of the 7th theoretical plate. Column 1 operated at a reflux value of 12 and a column top temperature of 40 ° C. The side stream 13, having a boiling range from 50 to 120 ° C, was withdrawn from the level of the 8th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 15 at the level of the 8th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to the ethanol separation column 3 having a theoretical plate number of 20 at the level of the 9th theoretical plate. Column 3 operated at a reflux value of 10 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. The methanol / acetone mixture stream 17 was fed to an extractive distillation column 6 having a number of theoretical plates 20 at the level of the 12th theoretical plate, and water 23 was added together as a solvent at the level of the 5th theoretical plate. Column 6 was operated at a weight ratio of solvent to stream 17 of 10, a reflux ratio of 9, and a column top temperature of 56 to 56.5 ° C. to obtain acetone 24 as a distillate from the top of the column and to obtain a mixture of 25 methanol / solvent from the bottom of the column . A mixture of 25 methanol / solvent was fed to the solvent regeneration column 7 having the number of theoretical plates 10 at the level of the 5th theoretical plate. Column 7 operated at a reflux value of 6 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 28 as a distillate from the top of the column and to obtain a regenerated solvent 29 from the bottom of the column. Stream 18 from the ethanol separation column was fed to the ethanol removal column 8, having the number of theoretical plates 15, at the level of the 10th theoretical plate, and column 8 was operated at a reflux value of 8 and a top temperature of the column from 68 to 68.5 ° C. to obtain ethanol 26 as a distillate from the top of the column and an aqueous solution of n-propanol 27 from the bottom of the column. An aqueous solution of n-propanol 27 was fed to the azeotropic distillation column 9, having a number of theoretical plates of 20, at the level of the 12th theoretical plate, and cyclohexane was simultaneously supplied as an azeotropic agent. In column 9, the weight ratio of the azeotropically forming agent to the aqueous solution of n-propanol 27 was 0.9, and the temperature of the bottom of the column was from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 30, and by refluxing from the oil phase, and with the removal of n-propanol 31 from the bottom of the column. A stream 15 from the acetic acid separation column 2 was supplied to the acetic acid extraction column 4 having the number of theoretical plates 10, and tert-butylamine was added together as an extraction reagent. Column 4 was operated at a weight ratio of extraction reagent to stream 15 of 5 and an operating temperature of 35 ° C, to obtain a mixture of 19 acetic acid / extraction reagent from the top of the column and to obtain wastewater 22 from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was fed into the extraction reagent regeneration column 5 having the number of theoretical plates 10 at the level of the 4th theoretical plate, and the column 5 was operated at a reflux value of 6 and a column top temperature of 115 to 118 ° C. to obtain acetic acid 20 as a distillate from the top of the column, and to obtain a regenerated extracting reagent 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 6.

Table 6
Analytical data (weight percent) for flows of individual columns

Example 7

As shown in Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1, having the number of theoretical plates 60, at the level of the 35th theoretical plate. Column 1 operated at a reflux value of 1 and a column top temperature of 40 ° C. Side run 13, having a boiling point range from 50 to 120 ° C, was taken out from the level of the 40th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 50 at the level of the 30th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to ethanol separation column 3 having a theoretical plate number of 80 at the level of the 50th theoretical plate. Column 3 operated at a reflux value of 2 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. The methanol / acetone mixture stream 17 was fed to an extractive distillation column 6 having a theoretical plate number of 50 at the level of the 20th theoretical plate, and monoethanolamine 23 was supplied together as a solvent at the level of the 3rd theoretical plate. Column 6 was operated at a weight ratio of solvent to stream 17 of 2, a reflux ratio of 2, and a column top temperature of 56 to 56.5 ° C. to obtain acetone 24 as a distillate from the top of the column and a mixture of 25 methanol / solvent from the bottom of the column. A mixture of 25 methanol / solvent was fed to the solvent regeneration column 7 having a theoretical plate number of 50 at the level of the 20th theoretical plate. Column 7 operated at a reflux value of 1.5 and a top temperature of the column from 64.5 to 64.7 ° C, to obtain methanol 28 as a distillate from the top of the column and to obtain a regenerated solvent 29 from the bottom of the column. Stream 18 of an aqueous solution of ethanol and n-propanol from the ethanol separation column 3 was fed to the ethanol removal column 8 having a number of theoretical plates 60 at the level of the 40th theoretical plate. Column 8 operated at a reflux value of 2 and a top temperature of the column from 68 to 68.5 ° C, to obtain ethanol 26 as a distillate from the top of the column and an aqueous solution of n-propanol 27 from the bottom of the column. An aqueous solution of n-propanol 27 was fed to the azeotropic distillation column 9 having a theoretical plate number of 60 at the level of the 35th theoretical plate, and n-butyl acetate was introduced together as an azeotropic agent. In column 9, the weight ratio of the azeotropically forming agent to the aqueous solution of n-propanol 27 was 0.2, and the temperature of the bottom of the column was from 96.8 to 97.5 ° C, with the withdrawal of the aqueous phase obtained in the phase separator of the top of the column as stream 30, and by refluxing from the oil phase, and with the removal of n-propanol 31 from the bottom of the column. Stream 15 of an aqueous solution of acetic acid from the acetic acid separation column 2 was supplied to the acetic acid extraction column 4 having 40 theoretical plates, and n-butylamine was added together as an extraction reagent. Column 4 was operated at a weight ratio of extraction reagent to stream 15 equal to 1 and an operating temperature of 35 ° C, to obtain a mixture of 19 acetic acid / extraction reagent from the top of the column and to obtain wastewater 22 from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was fed into the recovery reagent recovery column 5 having a theoretical plate number of 50 at the level of the 20th theoretical plate, and column 5 was operated at a reflux value of 1 and a column top temperature of 115 to 118 ° C. to obtain acetic acid acid 20 as a distillate from the top of the column and to obtain a regenerated extracting reagent 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 7.

Table 7
Analytical data (weight percent) for flows of individual columns

Example 8

As shown in Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1, having the number of theoretical plates 30, at the level of the 17th theoretical plate. Column 1 operated at a reflux value of 3 and a column top temperature of 40 ° C. The side stream 13, having a boiling range of 50 to 120 ° C, was taken out from the level of the 20th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 30 at the level of the 17th theoretical plate. Column 2 operated at a reflux value of 4 and a bottom temperature of the column from 104 to 108 ° C, obtaining a stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column and a stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to ethanol separation column 3 having a theoretical plate number of 40 at the level of the 25th theoretical plate. Column 3 operated at a reflux value of 4 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream of 18 aqueous solution of ethanol and n-propanol from the bottom of the column. The methanol / acetone mixture stream 17 was fed to an extractive distillation column 6 having a number of theoretical plates 30 at the level of the 17th theoretical plate, and ethylene glycol 23 was supplied together as a solvent at the level of the 3rd theoretical plate. Column 6 was operated at a weight ratio of solvent to stream 17 of 4, a reflux ratio of 4, and a column top temperature of 56 to 56.5 ° C. to obtain acetone 24 as a distillate from the top of the column and a mixture of 25 methanol / solvent from the bottom of the column. A mixture of 25 methanol / solvent was fed into the solvent regeneration column 7 having the number of theoretical plates 25 at the level of the 10th theoretical plate. Column 7 was operated at a reflux value of 3 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 28 as a distillate from the top of the column and to obtain a regenerated solvent 29 from the bottom of the column. Stream 18 of an aqueous solution of ethanol and n-propanol from the ethanol separation column was fed to the ethanol removal column 8 having a number of theoretical plates 30 at the level of the 20th theoretical plate. Column 8 operated at a reflux value of 4 and a top temperature of the column from 68 to 68.5 ° C, to obtain ethanol 26 as a distillate from the top of the column and to obtain an aqueous solution of n-propanol 27 from the bottom of the column. An aqueous solution of n-propanol 27 was fed to the azeotropic distillation column 9, having the number of theoretical plates 30, at the level of the 17th theoretical plate, and isopropyl acetate was introduced together as an azeotropic agent. In column 9, the weight ratio of the azeotropically forming agent to the aqueous solution of n-propanol 27 was 0.5, and the temperature of the bottom of the column was from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 30, and by refluxing from the oil phase, and with the removal of n-propanol 31 from the bottom of the column. Stream 15 of an aqueous solution of acetic acid from the acetic acid separation column 2 was supplied to the acetic acid extraction column 4 having a theoretical number of plates 20, and trimethylphosphine oxide was added together as an extraction reagent. Column 4 was operated at a weight ratio of extraction reagent to stream 15 equal to 2 and an operating temperature of 35 ° C, to obtain a mixture of 19 acetic acid / extraction reagent from the top of the column and to obtain wastewater 22 from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was fed into the recovery reagent recovery column 5 having a theoretical plate number of 25 at the level of the 10th theoretical plate, and column 5 was operated at a reflux value of 3 and a column top temperature of 115 to 118 ° C. to produce acetic acid 20 as a distillate from the top of the column and to obtain a regenerated extracting reagent 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 8.

Table 8
Analytical data (weight percent) for flows
individual columns

Example 9

The procedure was followed as described in Example 8, except that triphenylphosphine oxide was used as the extraction reagent in the acetic acid extraction column 4. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 9.

Table 9
Analytical data (weight percent) for flows of individual columns

Example 10

The procedure was followed as described in Example 8, except that the by-products in the aqueous phase of the Fischer-Tropsch synthesis had the composition: 7 weight percent of a component having a boiling point of less than 50 ° C, 84 weight percent of a component having a boiling range of 50 to 120 ° C, and 9 weight percent of a component having a boiling point of more than 120 ° C. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 10.

Table 10
Analytical data (weight percent) for flows of individual columns

Example 11

As shown in Figure 3, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates of 15 at the level of the 7th theoretical plate. Column 201 operated at a reflux value of 12 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 8th theoretical plate. Side run 211 was fed to sectional column 202 having the number of theoretical plates 50, in which the number of theoretical plates 10 fell on the upper section, the number of theoretical plates 10 also fell on the lower section, the liquid phase of the left side in the upper section had a distribution coefficient of 0.7, and the gas phase of the left side in the lower section had a distribution coefficient of 0.68. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. Stream 214 of an aqueous solution of n-propanol was supplied to an azeotropic distillation column 203 having a number of theoretical plates 20 at the level of the 12th theoretical plate, and cyclohexane was simultaneously supplied as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.9, and the bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. Stream 215 of an aqueous solution of acetic acid from section column 202 was supplied to acetic acid extraction column 204 having a number of theoretical plates 10, and tert-butylamine was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 5 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extracting reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a number of theoretical plates 10 at the level of the 4th theoretical plate. Column 205 operated at a reflux value of 6 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column and to produce a regenerated extractant 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 11.

Table 11
Analytical data (weight percent) for flows of individual columns

Example 12

As shown in Figure 3, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates 60 at the level of the 35th theoretical plate. Column 201 operated at a reflux value of 1 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 40th theoretical plate. The side strap 211 was fed to a sectional column 202 having a number of theoretical plates 200, in which the number of theoretical plates 40 was in the upper section, the number of theoretical plates was 60 in the lower section, and the liquid phase of the left side in the upper section had a distribution coefficient of 0.31, and the gas phase of the left side in the lower section had a distribution coefficient of 0.3. Section column 202 operated at a reflux value of 30, a column top temperature of 60 to 64 ° C, an upper side stream temperature of 68 to 68.5 ° C and a lower side temperature of 87 to 93 ° C, with a mixture of 212 acetone and methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the upper part of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from the bottom to olonni. Stream 214 of an aqueous solution of n-propanol was fed to an azeotropic distillation column 203 having a number of theoretical plates 60 at the level of the 35th theoretical plate, and n-butyl acetate was introduced together as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.2 and the bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. Stream 215 of an aqueous solution of acetic acid from section column 202 was fed to acetic acid extraction column 204 having a number of theoretical plates 40, and tert-butylamine was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 1 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extraction reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a theoretical plate number of 50 at the level of the 20th theoretical plate. Column 205 operated at a reflux value of 1 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column and to obtain a regenerated extracting reagent 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 12.

Table 12
Analytical data (weight percent) for flows of individual columns

Example 13

As shown in Figure 3, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates 30 at the level of the 17th theoretical plate. Column 201 operated at a reflux value of 3 and a column top temperature of 40 ° C, with a sidestream of 211 having a boiling point range of 50 to 120 ° C, from the level of the 20th theoretical plate. The side run 211 was fed to a sectional column 202 having a number of theoretical plates 120, in which the number of theoretical plates 20 fell on the upper section, the number of theoretical plates 30 fell on the lower section, the liquid phase of the left side in the upper section had a distribution coefficient of 0.52, and the gas phase of the left side in the lower section had a distribution coefficient of 0.5. Sectional column 202 operated at a reflux value of 12, a column top temperature of 60 to 64 ° C, an upper side stream temperature of 68 to 68.5 ° C and a lower side temperature of 87 to 93 ° C, with the mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. Stream 214 of an aqueous solution of n-propanol was supplied to an azeotropic distillation column 203 having a number of theoretical plates 30 at the level of the 17th theoretical plate, and isopropyl acetate was introduced together as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.5 and a bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. An aqueous solution of acetic acid 215 from the section column 202 was supplied to the acetic acid extraction column 204 having the number of theoretical plates 20, and trimethylphosphine oxide was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 2 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extracting reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a theoretical plate number of 25 at the level of the 10th theoretical plate. Column 205 operated at a reflux value of 3 and a top temperature of the column from 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column and to obtain a regenerated extractant 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 13.

Table 13
Analytical data (weight percent) for flows of individual columns

Example 14

The procedure was followed as described in Example 13, except that the by-products in the aqueous phase of the Fischer-Tropsch synthesis had the composition: 7 weight percent of a component having a boiling point of less than 50 ° C., 84 weight percent of a component having a boiling range of 50 to 120 ° C, and 9 weight percent of a component having a boiling point of more than 120 ° C. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 14.

Table 14
Analytical data (weight percent) for flows of individual columns

Example 15

As shown in Figure 4, stream 208 consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C., 85 weight percent of a component having a boiling point of 50 to 120 ° C., and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates of 15 at the level of the 7th theoretical plate. Column 201 operated at a reflux value of 12 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 8th theoretical plate. Side run 211 was fed to sectional column 202 having the number of theoretical plates 50, in which the number of theoretical plates 10 fell on the upper section, the number of theoretical plates 10 also fell on the lower section, the liquid phase of the left side in the upper section had a distribution coefficient of 0.7, and the gas phase of the left side in the lower section had a distribution coefficient of 0.68. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. A mixture of 212 acetone / methanol and water 223 as a solvent were fed into the extractive distillation column 206, having the number of theoretical plates 20, at the level of the 12th and 5th theoretical plates, respectively. Column 206 operated with a weight ratio of solvent to mixture of 212 acetone / methanol equal to 10, a reflux ratio of 9, and a top temperature of the column from 56 to 56.5 ° C to obtain acetone 224 as a distillate from the top of the column and a mixture of 225 methanol / solvent from the bottom of the column . A mixture of 225 methanol / solvent was fed to the solvent regeneration column 207 having the number of theoretical plates 10 at the level of the 5th theoretical plate. Column 207 was operated at a reflux value of 6 and a column top temperature of 64.5 to 64.7 ° C., to obtain methanol 226 as a distillate from the top of the column and to obtain a regenerated solvent 227 from the bottom of the column. An aqueous solution of n-propanol 214 from the section column 202 was fed to the azeotropic distillation column 203 having the number of theoretical plates 20 at the level of the 12th theoretical plate, and cyclohexane was added together as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.9, and the bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. An aqueous solution of acetic acid 215 from the section column 202 was fed to the acetic acid extraction column 204 having a number of theoretical plates 10, and tert-butylamine was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 5 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extracting reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a number of theoretical plates 10 at the level of the 4th theoretical plate. Column 205 operated at a reflux value of 6 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column and to produce a regenerated extractant 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 15.

Table 15
Analytical data (weight percent) for flows of individual columns

Example 16

As shown in Figure 4, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates 60 at the level of the 35th theoretical plate. Column 201 operated at a reflux value of 1 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 40th theoretical plate. The side strap 211 was fed to a sectional column 202 having a number of theoretical plates 200, in which the number of theoretical plates 40 was in the upper section, the number of theoretical plates was 60 in the lower section, and the liquid phase of the left side in the upper section had a distribution coefficient of 0.31, and the gas phase of the left side in the lower section had a distribution coefficient of 0.3. Sectional column 202 operated at a reflux value of 30, a column top temperature of 60 to 64 ° C, a temperature of the upper side stream from 68 to 68.5 ° C and a temperature of the lower side stream from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column, and to obtain an aqueous solution of acetic acid 215 from a low bosoms. A mixture of 212 acetone / methanol and monoethanolamine 223 as a solvent was fed into the extractive distillation column 206, having the number of theoretical plates 50, at the level of the 20th and 3rd theoretical plates, respectively. Column 206 operated with a weight ratio of solvent to mixture of 212 acetone / methanol equal to 2, a reflux value of 2, and a top temperature of the column from 56 to 56.5 ° C, to obtain acetone 224 as a distillate from the top of the column and to obtain a mixture of 225 methanol / solvent from the bottom of the column. A 225 methanol / solvent mixture was fed to a solvent regeneration column 207 having a number of theoretical plates 50 at the level of the 20th theoretical plate. Column 207 was operated at a reflux value of 1.5 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 226 as a distillate from the top of the column and to obtain a regenerated solvent 227 from the bottom of the column. An aqueous solution of n-propanol 214 from the section column 202 was supplied to the azeotropic distillation column 203 having the number of theoretical plates 60 at the level of the 35th theoretical plate, and n-butyl acetate was introduced together as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.2 and the bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. An aqueous solution of acetic acid 215 from the section column 202 was supplied to the acetic acid extraction column 204 having the number of theoretical plates 40, and tert-butylamine was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 1 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extracting reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a theoretical plate number of 50 at the level of the 20th theoretical plate. Column 205 operated at a reflux value of 1 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column, and to obtain a regenerated extractant 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 16.

Table 16
Analytical data (weight percent) for flows of individual columns

Example 17

As shown in Figure 4, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates 30 at the level of the 17th theoretical plate. Column 201 operated at a reflux value of 3 and a column top temperature of 40 ° C, with a sidestream of 211 having a boiling point range of 50 to 120 ° C, from the level of the 20th theoretical plate. The side run 211 was fed to a sectional column 202 having a number of theoretical plates 120, in which the number of theoretical plates 20 fell on the upper section, the number of theoretical plates 30 fell on the lower section, the liquid phase of the left side in the upper section had a distribution coefficient of 0.52, and the gas phase of the left side in the lower section had a distribution coefficient of 0.5. Sectional column 202 operated at a reflux value of 12, a column top temperature of 60 to 64 ° C, an upper side stream temperature of 68 to 68.5 ° C and a lower side temperature of 87 to 93 ° C, with the mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. A mixture of 212 acetone and methanol and ethylene glycol 223 as a solvent was fed to extractive distillation column 206, having the number of theoretical plates 30, at the level of the 17th and 3rd theoretical plates, respectively. Column 206 worked with a weight ratio of solvent to mixture of 212 acetone / methanol equal to 4, a reflux ratio of 4 and a top temperature of the column from 56 to 56.5 ° C, to obtain acetone 224 as a distillate from the top of the column and to obtain a mixture of 225 methanol / solvent from the bottom of the column. A 225 methanol / solvent mixture was fed to a solvent regeneration column 207 having a theoretical plate number of 25 at the level of the 10th theoretical plate. Column 207 was operated at a reflux value of 3 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 226 as a distillate from the top of the column and to obtain a regenerated solvent 227 from the bottom of the column. An aqueous solution of n-propanol 214 from the section column 202 was supplied to the azeotropic distillation column 203 having the number of theoretical plates 30 at the level of the 17th theoretical plate, and isopropyl acetate was added together as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.5 and a bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. An aqueous solution of acetic acid 215 from the section column 202 was supplied to the acetic acid extraction column 204 having the number of theoretical plates 20, and trimethylphosphine oxide was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 2 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extracting reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a theoretical plate number of 25 at the level of the 10th theoretical plate. Column 205 operated at a reflux value of 3 and a top temperature of the column from 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column and to obtain a regenerated extractant 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 17.

Table 17
Analytical data (weight percent) for flows of individual columns

Example 18

The procedure was followed as described in Example 17, except that the by-products in the aqueous phase of the Fischer-Tropsch synthesis had the composition: 7 weight percent of a component having a boiling point of less than 50 ° C., 84 weight percent of a component having a boiling range of 50 to 120 ° C, and 9 weight percent of a component having a boiling point of more than 120 ° C. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 18.

Table 18
Analytical data (weight percent) for flows of individual columns

Example 19

As shown in the part of Figure 1, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1, having the number of theoretical plates 60, at the level of the 35th theoretical plate, with the operation of column 1 at a reflux value of 1 and temperature th column top 40C. Side run 13, having a boiling point range from 50 to 120 ° C, was taken out from the level of the 40th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 50 at the level of the 30th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to ethanol separation column 3 having a theoretical plate number of 80 at the level of the 50th theoretical plate. The ethanol separation column 3 operated at a reflux value of 2 and a column top temperature of 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 19.

Table 19
Analytical data (weight percent) for flows of individual columns

Example 20

As shown in the portion of Figure 3, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was supplied to a standard distillation column 201 having a number of theoretical plates of 15 at the level of the 7th theoretical plate. Column 201 operated at a reflux value of 12 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 8th theoretical plate. Side run 211 was fed to sectional column 202 having the number of theoretical plates 50, in which the number of theoretical plates 10 fell on the upper section, the number of theoretical plates 10 also fell on the lower section, the liquid phase of the left side in the upper section had a distribution coefficient of 0.7, and the gas phase of the left side in the lower section had a distribution coefficient of 0.68. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 20.

Table 20
Analytical data (weight percent) for flows of individual columns

Example 21

As shown in the portion of Figure 3, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates 60 at the level of the 35th theoretical plate. Column 201 operated at a reflux value of 1 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 40th theoretical plate. The side run 211 was fed into a sectional column 202 having a number of theoretical plates 200, in which the number of theoretical plates 40 fell on the upper section, the number of theoretical plates 60 fell on the lower section, and the liquid phase of the left side in the upper section had a distribution coefficient of 0.31. and the gas phase of the left side in the lower section had a distribution coefficient of 0.3. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. Stream 214 of an aqueous solution of n-propanol was fed to an azeotropic distillation column 203 having a number of theoretical plates 60 at the level of the 35th theoretical plate, and n-butyl acetate was introduced together as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.2 and the bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 21.

Table 21
Analytical data (weight percent) for flows of individual columns

Example 22

As shown in the portion of Figure 4, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was supplied to a standard distillation column 201 having a number of theoretical plates of 15 at the level of the 7th theoretical plate. Column 201 operated at a reflux value of 12 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 8th theoretical plate. Side run 211 was fed to sectional column 202 having the number of theoretical plates 50, in which the number of theoretical plates 10 fell on the upper section, the number of theoretical plates 10 also fell on the lower section, the liquid phase of the left side in the upper section had a distribution coefficient of 0.7, and the gas phase of the left side in the lower section had a distribution coefficient of 0.68. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. An aqueous solution of acetic acid 215 was supplied to an acetic acid extraction column 204 having a theoretical number of plates of 10, and tert-butylamine was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 5 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extracting reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a number of theoretical plates 10 at the level of the 4th theoretical plate. Column 205 operated at a reflux value of 6 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column and to produce a regenerated extractant 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 22.

Table 22
Analytical data (weight percent) for flows of individual columns

Example 23

As shown in the portion of Figure 4, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates 60 at the level of the 35th theoretical plate. Column 201 operated at a reflux value of 1 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 40th theoretical plate. The side strap 211 was fed to a sectional column 202 having a number of theoretical plates 200, in which the number of theoretical plates 40 was in the upper section, the number of theoretical plates was 60 in the lower section, and the liquid phase of the left side in the upper section had a distribution coefficient of 0.31, and the gas phase of the left side in the lower section had a distribution coefficient of 0.3. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. A mixture of 212 acetone / methanol and monoethanolamine 223 as a solvent was fed into an extractive distillation column 206 having a number of theoretical plates of 50 at the level of the 20th and 3rd theoretical plates, respectively. Column 206 operated with a weight ratio of solvent to mixture of 212 acetone / methanol equal to 2, a reflux value of 2, and a top temperature of the column from 56 to 56.5 ° C, to obtain acetone 224 as a distillate from the top of the column and to obtain a mixture of 225 methanol / solvent from the bottom of the column. A 225 methanol / solvent mixture was fed to a solvent regeneration column 207 having a number of theoretical plates 50 at the level of the 20th theoretical plate. Column 207 was operated at a reflux value of 1.5 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 226 as a distillate from the top of the column and to obtain a regenerated solvent 227 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 23.

Table 23
Analytical data (weight percent) for flows of individual columns

Example 24

As shown in the portion of Figure 4, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was supplied to a standard distillation column 201 having a number of theoretical plates of 15 at the level of the 7th theoretical plate. Column 201 operated at a reflux value of 12 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 8th theoretical plate. Side run 211 was fed to sectional column 202 having the number of theoretical plates 50, in which the number of theoretical plates 10 fell on the upper section, the number of theoretical plates 10 also fell on the lower section, the liquid phase of the left side in the upper section had a distribution coefficient of 0.7, and the gas phase of the left side in the lower section had a distribution coefficient of 0.68. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. A mixture of 212 acetone / methanol and water 223 as a solvent were fed into the extractive distillation column 206, having the number of theoretical plates 20, at the level of the 12th and 5th theoretical plates, respectively. Column 206 worked with a weight ratio of solvent to mixture of 212 acetone / methanol equal to 10, a reflux ratio of 9 and a top temperature of the column from 56 to 56.5 ° C, to obtain acetone 224 as a distillate from the top of the column and a mixture of 225 methanol / solvent from the bottom the columns. A mixture of 225 methanol / solvent was fed to the solvent regeneration column 207 having the number of theoretical plates 10 at the level of the 5th theoretical plate. Column 207 was operated at a reflux value of 6 and a column top temperature of 64.5 to 64.7 ° C., to obtain methanol 226 as a distillate from the top of the column and to obtain a regenerated solvent 227 from the bottom of the column. An aqueous solution of n-propanol 214 from the section column 202 was fed to the azeotropic distillation column 203 having the number of theoretical plates 20 at the level of the 12th theoretical plate, and cyclohexane was added together as an azeotropic agent. Column 203 worked with a weight ratio of the azeotropically forming agent to stream 214 equal to 0.9, and the bottom temperature of the column from 96.8 to 97.5 ° C, with the removal of the aqueous phase obtained in the phase separator of the top of the column as stream 217, and reflux by oil phase, and with the removal of n-propanol 218 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 24.

Table 24
Analytical data (weight percent) for flows of individual columns

Example 25

As shown in the portion of Figure 4, stream 208, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling range of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 201 having a number of theoretical plates 60 at the level of the 35th theoretical plate. Column 201 operated at a reflux value of 1 and a column top temperature of 40 ° C, with a lateral shoulder strap 211 having a boiling point range of 50 to 120 ° C, from the level of the 40th theoretical plate. The side strap 211 was fed to a sectional column 202 having a number of theoretical plates 200, in which the number of theoretical plates 40 was in the upper section, the number of theoretical plates was 60 in the lower section, and the liquid phase of the left side in the upper section had a distribution coefficient of 0.31, and the gas phase of the left side in the lower section had a distribution coefficient of 0.3. Sectional column 202 operated at a reflux value of 30, a column top temperature from 60 to 64 ° C, an upper side stream temperature from 68 to 68.5 ° C and a lower side stream temperature from 87 to 93 ° C, with a mixture of 212 acetone / methanol being removed from the top as a distillate columns, with the removal of ethanol 213 as a side stream from the top of the section column, with the removal of the stream 214 of an aqueous solution of n-propanol as a side stream from the bottom of the section column and with the formation of an aqueous solution of acetic acid 215 from a low onny. A mixture of 212 acetone / methanol and monoethanolamine 223 as a solvent was fed into an extractive distillation column 206 having a number of theoretical plates of 50 at the level of the 20th and 3rd theoretical plates, respectively. Column 206 operated with a weight ratio of solvent to mixture of 212 acetone / methanol equal to 2, a reflux value of 2, and a top temperature of the column from 56 to 56.5 ° C, to obtain acetone 224 as a distillate from the top of the column and to obtain a mixture of 225 methanol / solvent from the bottom of the column. A 225 methanol / solvent mixture was fed to a solvent regeneration column 207 having a number of theoretical plates 50 at the level of the 20th theoretical plate. Column 207 was operated at a reflux value of 1.5 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 226 as a distillate from the top of the column and to obtain a regenerated solvent 227 from the bottom of the column. An aqueous solution of acetic acid 215 from the section column 202 was supplied to the acetic acid extraction column 204 having the number of theoretical plates 40, and tert-butylamine was added together as an extraction reagent. Column 204 was operated at a weight ratio of extraction reagent to an aqueous solution of acetic acid 215 equal to 1 and a working temperature of 35 ° C, to obtain a mixture of 219 acetic acid / extracting reagent from the top of the column and to obtain wastewater 220 from the bottom of the column. A mixture of 219 acetic acid / extraction reagent was fed to the recovery reagent recovery column 205 having a theoretical plate number of 50 at the level of the 20th theoretical plate. Column 205 operated at a reflux value of 1 and a column top temperature of 115 to 118 ° C, to obtain acetic acid 221 as a distillate from the top of the column and to obtain a regenerated extracting reagent 222 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 25.

Table 25
Analytical data (weight percent) for flows of individual columns

Example 26

As shown in the part of Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling point of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1 having a number of theoretical plates of 15, at the level of the 7th theoretical plate. Column 1 operated at a reflux value of 12 and a column top temperature of 40 ° C. The side stream 13, having a boiling range from 50 to 120 ° C, was withdrawn from the level of the 8th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 15 at the level of the 8th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to the ethanol separation column 3 having a theoretical plate number of 20 at the level of the 9th theoretical plate. Column 3 operated at a reflux value of 10 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. The methanol / acetone mixture stream 17 was fed to an extractive distillation column 6 having a number of theoretical plates 20 at the level of the 12th theoretical plate, and water 23 was added together as a solvent at the level of the 5th theoretical plate. Column 6 was operated at a weight ratio of solvent to stream 17 of 10, a reflux ratio of 9, and a column top temperature of 56 to 56.5 ° C. to obtain acetone 24 as a distillate from the top of the column and to obtain a mixture of 25 methanol / solvent from the bottom of the column . A mixture of 25 methanol / solvent was fed to the solvent regeneration column 7 having the number of theoretical plates 10 at the level of the 5th theoretical plate. Column 7 operated at a reflux value of 6 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 28 as a distillate from the top of the column and to obtain a regenerated solvent 29 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 26.

Table 26
Analytical data (weight percent) for flows of individual columns

Example 27

As shown in the part of Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling point of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed to a standard distillation column 1 having a number of theoretical plates of 60 at the level of the 35th theoretical plate. Column 1 operated at a reflux value of 1 and a column top temperature of 40 ° C. Side run 13, having a boiling point range from 50 to 120 ° C, was taken out from the level of the 40th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 50 at the level of the 30th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to ethanol separation column 3 having a theoretical plate number of 80 at the level of the 50th theoretical plate. Column 3 operated at a reflux value of 2 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. An aqueous solution of 18 ethanol and n-propanol was fed to an ethanol removal column 8 having a number of theoretical plates 60 at the level of the 40th theoretical plate. Column 8 operated at a reflux value of 2 and a top temperature of the column from 68 to 68.5 ° C, to obtain ethanol 26 as a distillate from the top of the column and to obtain an aqueous solution of n-propanol 27 from the bottom of the column. An aqueous solution of n-propanol 27 was fed to the azeotropic distillation column 9 having a theoretical plate number of 60 at the level of the 35th theoretical plate, and n-butyl acetate was introduced together as an azeotropic agent. In column 9, the weight ratio of the azeotropically forming agent to the aqueous solution of n-propanol 27 was 0.2, and the temperature of the bottom of the column was from 96.8 to 97.5 ° C, with the withdrawal of the aqueous phase obtained in the phase separator of the top of the column as stream 30, and by refluxing from the oil phase, and with the removal of n-propanol 31 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 27.

Table 27
Analytical data (weight percent) for flows of individual columns

Example 28

As shown in the part of Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling point of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed into a standard distillation column 1 having a number of theoretical plates of 15, at the level of the 7th theoretical plate. Column 1 operated at a reflux value of 12 and a column top temperature of 40 ° C. The side stream 13, having a boiling range from 50 to 120 ° C, was withdrawn from the level of the 8th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 15 at the level of the 8th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to the ethanol separation column 3 having a theoretical plate number of 20 at the level of the 9th theoretical plate. Column 3 operated at a reflux value of 10 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. The methanol / acetone mixture stream 17 was fed to an extractive distillation column 6 having a number of theoretical plates 20 at the level of the 12th theoretical plate, and water 23 was added together as a solvent at the level of the 5th theoretical plate. Column 6 was operated at a weight ratio of solvent to stream 17 of 10, a reflux ratio of 9, and a column top temperature of 56 to 56.5 ° C. to obtain acetone 24 as a distillate from the top of the column and to obtain a mixture of 25 methanol / solvent from the bottom of the column . A mixture of 25 methanol / solvent was fed to the solvent regeneration column 7 having the number of theoretical plates 10 at the level of the 5th theoretical plate. Column 7 operated at a reflux value of 6 and a column top temperature of 64.5 to 64.7 ° C, to obtain methanol 28 as a distillate from the top of the column and to obtain a regenerated solvent 29 from the bottom of the column. A stream 15 from the acetic acid separation column 2 was supplied to the acetic acid extraction column 4 having the number of theoretical plates 10, and tert-butylamine was added together as an extraction reagent. Column 4 was operated at a weight ratio of extraction reagent to stream 15 equal to 5 and a working temperature of 35 ° C, to obtain a mixture of 19 acetic acid / extraction reagent from the top of the column and to obtain wastewater 22 from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was fed to the extraction reagent regeneration column 5 having the number of theoretical plates 10 at the level of the 4th theoretical plate, and the column 5 was operated at a reflux value of 6 and a column top temperature of 115 to 118 ° C. to obtain acetic acid 20 as a distillate from the top of the column and to obtain a regenerated extracting reagent 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 28.

Table 28
Analytical data (weight percent) for flows of individual columns

Example 29

As shown in the part of Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling point of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed to a standard distillation column 1 having a number of theoretical plates of 60 at the level of the 35th theoretical plate. Column 1 operated at a reflux value of 1 and a column top temperature of 40 ° C. Side run 13, having a boiling point range from 50 to 120 ° C, was taken out from the level of the 40th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 50 at the level of the 30th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to ethanol separation column 3 having a theoretical plate number of 80 at the level of the 50th theoretical plate. Column 3 operated at a reflux value of 2 and a top temperature of the column from 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column and to obtain a stream 18 of an aqueous solution of ethanol and n-propanol from the bottom of the column. Stream 18 of an aqueous solution of ethanol and n-propanol from the ethanol separation column was fed to the ethanol removal column 8 having a number of theoretical plates 60 at the level of the 40th theoretical plate. Column 8 operated at a reflux value of 2 and a top temperature of the column from 68 to 68.5 ° C, to obtain ethanol 26 as a distillate from the top of the column and to obtain an aqueous solution of n-propanol 27 from the bottom of the column. An aqueous solution of n-propanol 27 was fed to the azeotropic distillation column 9 having a theoretical plate number of 60 at the level of the 35th theoretical plate, and n-butyl acetate was introduced together as an azeotropic agent. In column 9, the weight ratio of the azeotropically forming agent to the aqueous solution of n-propanol 27 was 0.2, and the temperature of the bottom of the column was from 96.8 to 97.5 ° C, with the withdrawal of the aqueous phase obtained in the phase separator of the top of the column as stream 30, and by refluxing from the oil phase, and with the removal of n-propanol 31 from the bottom of the column. Stream 15 of an aqueous solution of acetic acid from the acetic acid separation column 2 was supplied to the acetic acid extraction column 4 having 40 theoretical plates, and n-butylamine was added together as an extraction reagent. Column 4 was operated at a weight ratio of extraction reagent to stream 15 equal to 1 and an operating temperature of 35 ° C, to obtain a mixture of 19 acetic acid / extraction reagent from the top of the column, and to obtain wastewater 22 from the bottom of the column. A mixture of 19 acetic acid / extraction reagent was supplied to the extraction reagent regeneration column 5 having the number of theoretical plates 50 at the level of the 20th theoretical plate, and the column 5 was operated at a reflux value of 1 and a column top temperature of 115 to 118 ° C. to obtain acetic acid 20 as a distillate from the top of the column, and to obtain a regenerated extracting reagent 21 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 29.

Table 29
Analytical data (weight percent) for flows of individual columns

Example 30

As shown in the part of Figure 2, stream 10, consisting of by-products in the aqueous phase of the Fischer-Tropsch synthesis (comprising 5 weight percent of a component having a boiling point of less than 50 ° C, 85 weight percent of a component having a boiling point of 50 to 120 ° C, and 10 weight percent of a component having a boiling point of more than 120 ° C) was fed to a standard distillation column 1 having a number of theoretical plates of 60 at the level of the 35th theoretical plate. Column 1 operated at a reflux value of 1 and a column top temperature of 40 ° C. Side run 13, having a boiling point range from 50 to 120 ° C, was taken out from the level of the 40th theoretical plate and fed into the column 2 of the acetic acid separation having the number of theoretical plates 50 at the level of the 30th theoretical plate. Column 2 operated at a reflux value of 8 and a bottom temperature of the column from 104 to 108 ° C, to obtain stream 14 of an aqueous solution containing alcohols and ketones as distillate from the top of the column, and stream 15 of an aqueous solution of acetic acid obtained from the bottom of the column. Stream 14 was fed to ethanol separation column 3 having a theoretical plate number of 80 at the level of the 50th theoretical plate. Column 3 operated at a reflux value of 2 and a top temperature of the column of 60 to 64 ° C, to obtain a stream 17 of a methanol / acetone mixture as distillate from the top of the column, and to obtain a stream of 18 aqueous solution of ethanol and n-propanol from the bottom of the column. The methanol / acetone mixture stream 17 was fed to an extractive distillation column 6 having a theoretical plate number of 50 at the level of the 20th theoretical plate, and monoethanolamine 23 was supplied together as a solvent at the level of the 3rd theoretical plate. Column 6 was operated at a weight ratio of solvent to stream 17 of 2, a reflux ratio of 2, and a column top temperature of 56 to 56.5 ° C. to obtain acetone 24 as a distillate from the top of the column and to obtain a mixture of 25 methanol / solvent from the bottom of the column . A mixture of 25 methanol / solvent was fed to the solvent regeneration column 7 having a theoretical plate number of 50 at the level of the 20th theoretical plate. Column 7 operated at a reflux value of 1.5 and a top temperature of the column from 64.5 to 64.7 ° C, to obtain methanol 28 as a distillate from the top of the column and to obtain a regenerated solvent 29 from the bottom of the column. Stream 18 of an aqueous solution of ethanol and n-propanol from the ethanol separation column 3 was fed to the ethanol removal column 8 having a number of theoretical plates 60 at the level of the 40th theoretical plate. Column 8 operated at a reflux value of 2 and a top temperature of the column from 68 to 68.5 ° C, to obtain ethanol 26 as a distillate from the top of the column and to obtain an aqueous solution of n-propanol 27 from the bottom of the column. An aqueous solution of n-propanol 27 was fed to the azeotropic distillation column 9 having a theoretical plate number of 60 at the level of the 35th theoretical plate, and n-butyl acetate was introduced together as an azeotropic agent. In column 9, the weight ratio of the azeotropically forming agent to the aqueous solution of n-propanol 27 was 0.2, and the temperature of the bottom of the column was from 96.8 to 97.5 ° C, with the withdrawal of the aqueous phase obtained in the phase separator of the top of the column as stream 30, and by refluxing from the oil phase, and with the removal of n-propanol 31 from the bottom of the column. Under stable operating conditions, analytical data were obtained for flows of individual columns. The results are shown in Table 30.

Table 30
Analytical data (weight percent) for flows of individual columns

While the invention has been described with reference to exemplary embodiments, those skilled in the art will understand that various changes and modifications can be made without departing from the spirit and scope of the invention. Therefore, the invention is not limited to the specific embodiments disclosed as the best path considered for the implementation of the present invention, but the invention will include all embodiments falling within the scope of the attached claims.

Claims (9)

1. The method of separation of by-products in the aqueous phase of the Fischer-Tropsch synthesis, comprising stages
a) feeding the by-products in the aqueous phase to a standard distillation column in its middle part, with the withdrawal of a portion of stream I having a boiling range of 50 to 120 ° C. as a side stream, to obtain light components having a boiling point of less than 50 ° C, from the top of the column, and to obtain heavy components having boiling points higher than 120 ° C, from the bottom of the column; and
b) supplying stream I to one side of the section column in its middle part, removing stream II of methanol / acetone mixture as distillate from the top of the column, removing stream III of an aqueous solution of acetic acid from the bottom of the column, removing ethanol as a side stream from the top part of the opposite side, and with the removal of stream IV of an aqueous solution of n-propanol as a side stream from the bottom of the opposite side. 2. The method according to claim 1, in which the standard distillation column has a number of theoretical plates from 10 to 60, reflux ratio from 1 to 12 and the temperature of the top of the column is not less than 40 ° C; the sectional column has a number of theoretical plates from 50 to 200, in which 1/6 to 1/3 of the number of theoretical plates fall on the upper section, 1/6 to 1/3 of the number of theoretical plates fall on the lower section, the liquid phase of the feed side the upper section has a distribution coefficient from 0.3 to 0.7, the gas phase of the feed side in the lower section has a distribution coefficient from 0.3 to 0.7; and the sectional column has a reflux number from 5 to 30, a top temperature of the column from 60 to 64 ° C, an upper sidestream temperature from 68 to 68.5 ° C, and a lower sidestream temperature from 87 to 93 ° C. 3. The method according to claim 1, further comprising stages
c) supplying stream IV to the azeotropic distillation column in its middle part, and simultaneously supplying the azeotropically forming agent, with the removal of the aqueous phase obtained in the phase separator of the top of the column, and refluxing from the oil phase, and with the removal of n-propanol from the bottom of the column, in which the azeotropic the agent is at least one agent that forms an azeotropic mixture with a low boiling point with water. 4. The method according to claim 3, in which the azeotropic distillation column has a number of theoretical plates from 15 to 60, the weight ratio of the azeotropic agent to stream IV from 0.2 to 1, and the bottom temperature of the column from 96.8 to 97.5 ° C; and wherein the azeotropically forming agent is at least one selected from cyclohexane, benzene, toluene, isopropyl acetate and n-butyl acetate. 5. The method according to any one of claims 1 to 4, further comprising stages
d) supplying stream III to the top of the acetic acid extraction column and extraction reagent to the bottom of the column, discharging stream V of the mixture of acetic acid and extraction reagent from the top of the column and removing wastewater from the bottom of the column in which the extraction reagent is at least one a reagent selected from the group consisting of organic phosphines and organic amines; and
e) supplying stream V to the recovery column of the extraction reagent in its middle part, removing acetic acid as distillate from the top of the column and obtaining a regenerated extracting reagent from the bottom of the column. 6. The method according to claim 5, in which the column for the extraction of acetic acid has a number of theoretical plates from 10 to 40 and a weight ratio of extracting reagent to stream III from 1 to 6, and operates at normal temperature; the recovery agent recovery column has a number of theoretical plates from 10 to 50 and a reflux number from 1 to 6, and operates at atmospheric pressure or reduced pressure; and the extracting reagent is at least one reagent selected from the group consisting of three (C1-C6-alkyl) phosphine oxides, triphenylphosphine oxide, tert-butylamine, n-butylamine and tert-amylamine. 7. The method according to any one of claims 1 to 4, further comprising stages
f) feeding stream II to the extractive distillation column in its middle part and co-introducing the polar solvent into the column at its upper part to remove acetone as distillate from the top of the column and to obtain stream VI of a mixture of methanol and solvent from the bottom of the column; and
g) supplying stream VI to the solvent regeneration column in its middle part, removing methanol as a distillate from the top of the column and obtaining a regenerated solvent from the bottom of the column. 8. The method according to claim 7, in which the extractive distillation column has a number of theoretical plates from 20 to 50, the weight ratio of polar solvent to stream II from 2 to 10, the reflux ratio from 2 to 9, and the top temperature of the column from 56 to 56.5 ° C; the polar solvent is at least one solvent selected from the group consisting of water, ethylene glycol, N-formylmorpholine, tetramethylene sulfone and monoethanolamine; and the solvent regeneration column has a number of theoretical plates from 10 to 50, a reflux number from 1 to 6, and a top temperature of the column from 64.5 to 64.7 ° C. 9. The method according to claim 5, further comprising the steps of f) feeding stream II to the extractive distillation column in its middle part and co-supplying the polar solvent to the column in its upper part with the removal of acetone as distillate from the top of the column and obtaining stream VI of the mixture methanol and solvent from the bottom of the column; and g) feeding stream VI to the solvent regeneration column in its middle part, removing methanol as distillate from the top of the column and obtaining a regenerated solvent from the bottom of the column.

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