EA031141B1 - Method for fractionating an alcohol-containing liquid, and device for implementing the same - Google Patents

Abstract

The invention is related to fractionating distillation of alcohol-containing liquids in a centrifugal field and can be used to separate the ester-aldehyde fraction (EAF) together with intermediate mixtures. The source alcohol-containing liquid is divided in the device into two flows, one of which is set in rotary motion, and the second one is heated additionally to the alcohol-containing liquid boiling point and ejected through a random packing and a mesh to convert the liquid to a steam-gas-liquid emulsion; the emulsion is passed through a mesh in a centrifugal field to increase the inter-phase surface and to form ultrasonic waves; then it is fed to the rotating first flow of the alcohol-containing liquid, from which ester-aldehyde fraction and transient fractions in the form of floating bubbles with vapours of those fractions and gases dissolved in the alcohol-containing liquid are released. The device comprises a base 1 having a bubbler 2 with a thermometer 16 secured to it; a rotor drive 3; a top part of a stator 6 supported by legs (not shown); a steam separator 8 with a thermometer 17; an alcohol heater 9. A bubbler 2 is connected to the heater 9 and the steam separator 8 by a pipeline. Fastened to the top part of the bubbler 2 is a vapour extraction pipeline 22 connected to a released vapour condenser 10 provided with a condensate sensor 20 to which a condensate outlet pipeline 7 is connected. Also connected to the bubbler 2 is a transparent pipeline 12, one end of which is positioned opposite to the rotor 3, and the other above the top part of the stator 6. The rotor 3 consists of 2 disks connected to each other by vanes 4; at least one mesh 5 is placed on the inner parts of the vanes over the entire inside periphery of the rotor 1. The upper disk of the rotor 2 has an opening for passing the alcohol-containing liquid through a symmetrically disposed opening in the top part of the stator 6, a pipeline 13 connected to the bottom part of the tank of the steam separator 8 being secured to said symmetrically disposed opening. The group of inventions provides reduction of energy consumption.

Description

The invention relates to fractional distillation of an alcohol-containing liquid in a centrifugal field and can be used to separate the ether-aldehyde fraction (EAF) together with intermediate impurities. The original alcohol-containing liquid is divided into two streams in the installation, one of which is driven into rotation, and the second is further heated to the boiling point of the alcohol-containing liquid and ejected through

031141 Bl

031141 B1 disordered nozzle and grid, transferring liquid to vapor-gas-liquid emulsion, which is passed through a grid in a centrifugal field to increase the interfacial surface and the formation of ultrasonic waves and fed to a rotating first stream of alcohol-containing liquid, from which ether-aldehyde and transitional fractions are removed in the form of floating bubbles with vapor of these fractions and gases dissolved in an alcohol-containing liquid. The device consists of a base 1, to which a bubbler 2 is attached with a thermometer 16; drive rotor 3; the upper part of the stator 6 with the help of conventionally not shown legs; steam trap 8 with thermometer 17; alcohol heater 9. A bubbler 2 is connected by a pipeline with a heater 9 and a steam trap 8. To the upper part of the bubbler 2 a vapor extraction line 22 is attached, connected to a condenser of separated vapors 10, equipped with a condensate sensor 20 to which the condensate outlet pipe 7 is connected. a transparent pipeline 12 is connected, one end of which is located opposite the rotor 3, and the second over the top of the stator 6. The rotor 3 consists of 2 disks interconnected by blades 4, on the inside of which over the entire inner perimeter of the rotor 1, at least one grid 5 is superimposed. The upper disk of the rotor 2 has an opening for the passage of alcohol-containing liquid through a symmetrically located opening in the upper part of the stator 6, to which a pipe 13 is attached, connected to the lower part of the steam trap 8. A group inventions provides reduced power consumption.

The invention relates to fractional distillation of an alcohol-containing liquid in a centrifugal field and can be used to separate the ether-aldehyde fraction (EAF) together with intermediate impurities from an alcohol-containing liquid in the production of alcohol-containing products.

In the description of the invention, it is assumed that the alcohol-containing liquid contains the following conditionally separated fractions: head (ether-aldehyde), ethyl, transitional (isopropanol and crotonaldehyde), terminal (methyl).

The known method and device for separating low-boiling fractions from water and its degassing using a cavitation apparatus containing a stator, a rotor, a system for supplying and discharging a liquid [1].

The disadvantage of this method and device is the need for long-term recirculation of the treated water, which leads to its heating and excessive energy consumption, and there is no possibility of collecting and subsequent removal of vapors and gases.

The closest in technical essence to the claimed technical solution is a method of separation of water-organic mixtures and a device for its implementation, selected as a prototype for the method and device [2].

The method of separating the alcohol-containing liquid into fractions of the prototype involves heating the original alcohol-containing liquid, separating it in a centrifugal field into fractions, converting part of the fractions into a vaporous state and separating them from the remaining fractions in a liquid state, condensing vapor and withdrawing from the system the separated liquid flows from different factions.

The disadvantage of this method is high energy consumption. This is due to the fact that the separation of the original alcohol-containing liquid into fractions is achieved due to its heating with specially prepared water vapor. When this happens, water vapor is saturated with lightly boiling fractions of an alcohol-containing liquid, which are then separated from each other by means of a compressor and a membrane.

A device for the separation of alcohol-containing liquid into fractions of the prototype consists of a centrifugal apparatus, a heater (boiler), a condenser (cooler), a piping system, input and output media from the system. The centrifugal apparatus consists of a body inside which a rotor is fixed on the central axis, having the form of a vertical thin-walled cylinder, inside which concentric partitions are fixed, forming a zigzag space for the movement of water and steam.

The disadvantage of the device prototype is the complexity of the design.

An object of the invention is to develop a method for separating an alcohol-containing liquid into fractions at lower power consumption and simplifying the design of the device for its implementation.

The technical result is achieved by developing a new method for separating an alcohol-containing liquid into fractions at lower power consumption without additional use of water vapor to extract individual fractions from the liquid and convert them into steam and a device in which the rotor design is simplified and there is no compressor, membrane unit, or reboiler condenser.

A new method of separating an alcohol-containing liquid into fractions includes heating the original alcohol-containing liquid, separating it in a centrifugal field into fractions by converting part of the fractions into a vaporous state, separating the vapor, condensing the vapor and withdrawing separate streams of condensate and liquid from different fractions from the system.

The technical result for the method is achieved due to the following distinctive essential features: the initial alcohol-containing liquid is divided into two streams in the installation, one of which is driven into rotational motion, and the second is additionally heated to the boiling point of the alcohol-containing liquid and ejected through an irregular nozzle and grid, translating the liquid into vapor-gas-liquid emulsion, which is passed through a grid in the centrifugal field to increase the interfacial surface and form ultrasonic waves and odayut the rotating first liquid alcohol-containing stream from which output and transitional efiroaldegidnuyu fraction as blown bubble with pairs of these fractions and dissolved in the liquid alcohol-containing gases. The rotor is rotated at the speed required to obtain a vapor-liquid-liquid emulsion entering the inside of the rotor, and the temperature of the alcohol-containing liquid in the bubbler is maintained below the boiling point of ethanol by controlling the speed of rotation of the rotor. When dissolved gases are removed from an alcohol-containing liquid, incl. oxygen, which ensures its deaeration.

The claimed method is illustrated by the scheme (Fig. 1) in Appendix 1. The claimed method is implemented through a device consisting of a centrifugal apparatus, a heater, a condenser, a piping system, a liquid in and out.

The technical result for the device is achieved by the following distinctive essential features: the centrifugal apparatus is placed in a bubbler and consists of a stator, to which a heated alcohol-containing liquid passing through an unregulated nozzle and a grid in this pipeline and a hollow rotor consisting of Of the 2 disks connected along the edge between the blades, the inner part of which overlaps the entire inner perimeter of the rotor, at least one with yok The bubbler is connected by a pipe - 1 031141 wire with a heater and a steam trap. The steam separator is connected by pipeline with a condenser, a condensate sensor and a bubbler. The bubbler is connected by a pipeline to a condenser of exhausted vapors and gases, which is connected by a pipeline to a condensate sensor. Thermometers are built into the bubbler and steam trap to control the temperature of the alcohol-containing liquid. For visual control of the cavitation process, a transparent pipeline is used.

The design of the device is shown in FIG. 1 (Appendix 1).

FIG. 1 marked:

- base;

- bubbler;

- rotor;

- rotor blades;

- rotor mesh;

- the upper part of the stator of the rotor 3;

- condensate outlet pipe;

- steam trap;

- heater;

- condensed vapors condenser;

- condenser of vapors released during heating;

- the pipeline is transparent;

- pipeline for supplying heated fluid;

- pipeline condensate;

- pipeline supplying vapor;

- thermometer in the bubbler;

- thermometer in the steam trap;

- disordered nozzle;

- grid;

- condensate sensor;

- condensate sensor;

- vapor recovery pipeline;

- I / O fluid.

The device (Fig. 1) consists of a base 1, to which a bubbler 2 is attached with a thermometer 16; drive rotor 3; the upper part of the stator 6 with the help of conventionally not shown legs; steam trap 8 with thermometer 17; alcohol heater 9. A bubbler 2 is connected by a pipeline with a heater 9 and a steam trap 8. To the upper part of the bubbler 2 a vapor extraction line 22 is attached, connected to a condenser of separated vapors 10, equipped with a condensate sensor 20 to which the condensate outlet pipe 7 is connected. connected transparent pipe 12, one end of which is located opposite the rotor 3, and the second above the upper part of the stator 6.

The rotor 3 consists of 2 discs interconnected by blades 4, on the inside of which along the entire inner perimeter of the rotor 1 at least one grid 5 is superimposed. the stator 6, which is attached to the pipe 13 connected to the bottom of the tank of the steam trap 8.

The upper part of the steam separator 8 is connected to a pipe 15, the second end of which is connected to a vapor condenser released during heating 11, which in turn is connected to a condensate sensor 21 and a pipe 14, the second end of which is connected to a bubbler 2.

The method is carried out through the device as follows: the original alcohol-containing liquid is heated using waste heat to the specified temperatures (shown in the examples) and poured through the inlet 23 into the bubbler 2 to 2/3 of the tank height. When this alcohol-containing liquid is filled with a steam trap 8 and the heater pipe 9. The alcohol-containing liquid in the preheater 9 is heated by passing hot water through an existing jacket. The rotor drive 3 is turned on at a speed sufficient to form a vapor-gas-liquid emulsion controlled through a transparent pipe 12. The rotor blades 4, located along the edges of the rotor disks 3, rotate the alcohol-containing liquid in the bubbler 2. A vacuum is formed inside the rotor 3 due to the centrifugal field and the heated alcohol-containing liquid through pipe 13 begins to flow from the steam separator 8 to the stator 6, which has an opening closed by a grid 19, above which an unordered nozzle is located 18.

With the passage of an alcohol-containing liquid through the disordered nozzle 18, under the action of vacuum and cavitation arising, bubbles of dissolved gases and bubbles with EAF vapors and other fractions contained in the distilled alcohol-containing liquid begin to precipitate. And with the passage of the grid 19, the process of release of EAF gases and vapors into bubbles is accelerated, forming a stream of vapor-liquid-liquid emulsion. The flow of the vapor-gas-liquid emulsion from the stator 6 through symmetrically located holes rushes into the space between the disks of the rotor 3, where the center

- 2 031141 field and a vacuum is formed. The magnitude of the vacuum depends on the speed of rotation of the rotor. When the boiling point of the individual fractions is lowered, the alcohol-containing mixture decreases. As a result, the rate of formation of bubbles with steam from the EAF increases. The bubbles increase in size due to the evaporation of aldehydes, the volatility of which increases under the action of rarefaction. At the same time, the intermediate and other fractions evaporate. Next, the flow of this vapor-liquid emulsion collides with the grids 5 of the rotor 3 and enters the centrifugal field through the free space of the blades 4 into the primary rotating flow of alcohol-containing liquid in the bubbler 2, which is under atmospheric pressure. When a vapor-gas-liquid emulsion collides and passes through the grids 5, the interfacial surface increases, a part of the bubbles collapses, forming ultrasonic waves acting on the alcohol-containing liquid rotating in the bubbler 2. The collapse of bubbles also contributes to the fact that they enter the area of higher pressure. As a result of the interaction of ultrasonic waves with the vapor-liquid emulsion coming from the rotor 3, the surface of the bubbles is curved, which further increases the surface of the contact of the vapor with the liquid, as well as heat and mass transfer. At the same time, the bubbles, being in a turbulized liquid, rise to the top of the fluid layer due to the Archimedean force. This increases the contact time, which also affects condensation and the transfer of vapor to liquid. A rotating stream of alcohol-containing liquid and a stream of vapor-gas-liquid emulsion rising to the top (bubbling) increase the contact surface between the vapor and the liquid. In the interaction of liquid and vapor, heat and mass transfer occurs, as a result of which the temperature is equalized. The amount of released vapors depends on the vacuum inside the rotor, which in turn depends on the speed of its rotation, which determines the temperature of the alcohol-containing liquid in the bubbler 2.

Thus, due to heat and mass transfer, vapors of the liquid remain in the bubbles, the boiling point of which is lower than the boiling point of the liquid in the bubbler 2. The temperature of the distilled alcohol-containing liquid in the bubbler 2 is maintained by controlling the speed of rotation of the rotor 3, since at higher rotational speeds, a higher vacuum is created and, accordingly, more vapors are emitted, as a result of which the temperature of the liquid in the bubbler 2 decreases. This translates into bubbles with vapor of EAF and intermediate fractions, the remaining fractions remain in the liquid state.

The bubbles of the vapor-liquid emulsion in the bubbler 2 rise and burst in the funnel caused by the rotation of the alcohol-containing liquid. So over the surface of the funnel accumulate a pair of EAF and intermediate fractions and dissolved in an alcohol-containing liquid gases. Next, steam and gas flows through line 22 to condenser 10. After condensation of vapor in condenser 10, condensate is discharged through line 7 to the tank for further processing. The amount of condensate is measured by the flow meter 20. When the alcohol-containing liquid is heated in the preheater 9, alcohol vapors with ethanol may occur, which should not flow to the rotor 3. These vapors are fed through the pipe 15 to the condenser 11. Next, the condensed liquid is measured by the flow meter 21 and drained into the bubbler

2

During the installation, the alcohol-containing liquid from the bubbler 2 constantly enters the steam separator 8, from it into the heater 9, from which via line 13 to the stator 6. Next, passing through the uncontrolled nozzle 18 and the grids 19 and 5, turns into a vapor-liquid-liquid emulsion, where in vapor bubbles contains EAF and gases. The alcohol-containing liquid purified in this way from EAF and dissolved gases is discharged through terminal 23 into a special container for further processing.

The control of the technological process is carried out by monitoring the temperatures with thermometers 16 and 17 and a visual sensor 12 (pipeline with a transparent window). If the process of separation of fractions has begun, then a stream of bubbles is viewed through the window.

The inventive method has passed pilot tests in a pilot laboratory installation. Example 1

A check was made on the possibility of separating EAF from the head fraction concentrate, which is formed during the preparation of pure ethyl alcohol. For this purpose, the device shown in FIG. 1 with the following characteristics: the bubbler 2 has a diameter of 140 mm, a height of 250 mm; diameter of rotor 3 is 70 mm, height between rotor disks is 9 mm, inlet 12 mm, electric drive power 0.5 kW, number of nets 5-3 pcs. with a gap between them 1 mm. In the bubbler 2 through the input-output device 23 was filled with alcohol-containing liquid containing concentrate head fraction with a strength of 40% ab with a preheating temperature of 70 ° C. This alcohol-containing liquid also filled the pipeline with the heater 9 and the steam separator 8, the internal cavity of the rotor 3 and the pipeline 13. The heater of the heater 9 and the drive of the rotor 3 were turned on, setting the speed to 6000 rpm. During the rotation of the rotor 3, the blades 4 cause the alcohol-containing liquid to rotate in the bubbler 2 and the cavity of the rotor 3. Due to the rotation of the rotor 3, a vacuum is formed at its entrance and in the stator 6. The gap between the rotor 3 and the stator is 6-1.5 mm. Under the action of dilution, an alcohol-containing liquid through a pipeline 13 with a diameter of 20 mm, having a diaphragm with an opening of 4 mm at the outlet, flows from the steam separator 8 to the stator 6 through an unordered nozzle 18 and a grid 19 with a cell size of 0.1 x 0.1 mm, thus forming a stream of distilled alcohol-containing liquids with a capacity of 2-2.5 l / min. With the passage through the disordered nozzle 18 and the grid 19 alcohol-containing

- 3 031141 the liquid is filtered, cavitates and gets inside the rotor 3: at the beginning of the distillation in the form of a gas-liquid flow, and when it reaches 76 ° C vapor-gas-liquid flow. At the same time at the exit of the pipeline 7 appears liquid. After 10 minutes of distillation, the temperature in the bubbler 2 rose to 81 ° C, and in the steam trap 8 to 83 ° C.

After pouring the alcohol-containing liquid from the bubbler 2, sample 1 was taken and sent for chromatographic analysis (Appendix 2).

After distillation of the alcohol-containing liquid, sample 2 was taken and sent for chromatographic analysis (Appendix 3).

The data are given in the table.

Title Inlet mg / L (K) Output mg / L (KI) K / Kl Acetaldehyde (Acetaldehude) 889.311 109.741 8.1 Methyl acetate (Methylacetate) 162.278 30.769 5.2 Ethyl acetate (Ethylacetate) 4484.790 1070.140 4.2 Methanol (Methanol) 0.108 0.0981 1.1 Isopropanol (i-propanol) 46.74 missing missing η-propanol (n-Propanol) 7556.942 6105.184 1.2 Krotonaldehyde (Krotonaldehude) 9.388 missing missing Isobutanol (i-Butanol) 20233.51 17961.66 1.1 n-Butanol (n-Butanol) 67.724 58.3 1.2 Isoamilol (i- Ami lol) 15675.61 13670.32 1.2

Analysis of the data shows the complete absence after purification of the claimed method of isopropanol and crotonaldehyde, a significant decrease in impurities such as acetaldehyde, methyl acetate, ethyl acetate.

Example 2

Vodka having a specific odor was used as a distilled alcohol-containing liquid in order to separate the fractions, giving it this smell, as well as residues from the EAF. In the process of distillation the device was used (Fig. 1). In the bubbler 2 pre-heated vodka was poured to a temperature of 70 ° C with a strength of 40% ab. After the apparatus was put into operation, the temperature in the bubbler 2 and the steam separator 8 began to grow and after reaching the temperature in the bubbler 2 76 ° C, liquid 7 appeared from the pipeline 7 with a strong odor of distilled vodka, which was maintained until 10-12 drops in the bubbler temperature process. After reaching a temperature of 78 ° C, the distillation was completed. At the same time, the presence of bubbles in the control transparent pipeline 12 was maintained from the beginning of the start of the apparatus for distillation. After processing, its strength decreased by 1.5% ab, the smell disappeared, and its taste properties improved significantly. The hangover syndrome was virtually absent.

Thus the problem is solved. The technical result is achieved. A new method of separating an alcohol-containing liquid into fractions is less energy-consuming. The design of the device for implementing a new method for separating an alcohol-containing liquid into fractions is much simplified.

Sources

1) The patent for the invention of the Russian Federation RU 2259322 Water dearatation method, published on August 27, 2005 - (analogues)

2) A patent for the invention of the Russian Federation RU 2489198 A method for the separation of water-organic mixtures and a device for its implementation, published on 10.08.2013 (prototype).

Claims (6)

CLAIM 1. A method of separating an alcohol-containing liquid into fractions, including heating the original alcohol-containing liquid, separating it in a centrifugal field into fractions by converting part of the fractions into a vaporous state, separating vapor, condensation of vapors and output from the system of separated streams of condensate and liquid with different fractions, characterized by that the initial alcohol-containing liquid is divided into two streams in the installation, one of which is set in rotational motion, and the second is additionally heated to the boiling point of alcohol containing liquid and ejected through the disordered nozzle and the grid, transferring the liquid into a vapor-liquid-liquid emulsion, which is passed through the grid in the centrifugal field to increase the interfacial surface and form ultrasonic waves and fed into the rotating first stream of alcohol-containing liquid, from which the ether-aldehyde and transition fractions are removed as a spray bubbles with 2. The method according to claim 1, characterized in that the rotor is rotated at a speed necessary to obtain a vapor-liquid emulsion entering the inside of the rotor. 3. The method according to claim 1, characterized in that the temperature of the alcohol-containing liquid in the bubbler is maintained below the boiling point of ethanol by controlling the speed of rotation of the rotor. 4. A device for the separation of alcohol-containing liquid into fractions by the method according to claim 1, consisting of a centrifugal apparatus, a heater, a condenser, a piping system, input and output of fluids from the system, characterized in that the rotor and stator of the centrifugal apparatus are placed in a bubbler, and the lower part the bubbler is connected by a pipeline with a heater and a steam separator, and a vapor removal pipeline with a condenser and a condensate sensor and a condensate removal pipeline with a condenser and a condensate sensor are attached to its upper part, A pipe connected to a steam trap, which is connected to the stator with a disordered nozzle with a grid, inside which the rotor rotates, consisting of two disks connected at the edges of the blades, on the inside of which overlap at least one grid, on the inside of the rotor, opposite which is located one entrance to the transparent pipeline, and its output is located above the upper part of the stator. FIG. one External Standard Report Data File Name: C: \ PROGRA ~ 1 \ BELHARD \ i \ data \ s: IVUHA \ NV-Fa968. D Operator Page Number: one Instrument : ANALYZER1 Vial Number: Sample Name : KGF ISH Injection Number: Run time bar Code: Sequence Line: Acquired on : 02 Feb 10 12:35 PM Instrument Method: SIVUHA.MTH Report Created on: 02 Feb 10 01:19 PM Analysis Method: SIVUHA.MTH Last recalib on: 02 Feb 10 08:38 AM Sample Amount: 0 Multiplier : one ISTD Amount: Sig. 1 in C: ' \ PROGRA-1 \ BELHARD \ 1 \ DATA \ S IVUHA \ NV-i Fa968.D Ret time Area type Width Ref # mg / L Name A ₍ '6.019 * 31090 * BB 0.035 1 889.311 Acetaldehude 7.041 5256 VB 0.051 1 162.278 Methylacetate 8.001 191281 W 0.053 1 4484.790 Ethylacetate 8.215 35688 VB 0.053 1 0.108 Methanol i 8.768 12.543 2543 BV 513901 BB 0.089 1 0.078 1 46.746 7556.942 i-Propanol - „ n-propanol 13.585 4 96 EM 0.095 1 9.388 Krotonaldehude - - 14.734 1708466 BB 0.100 1 20233.51 i-Butanol -t-rfii λ ί 17.134 5410 BB 0.076 1 67.724 n-Butanol 5X 3 A 4. 19.620 1465351 VB 0.098 1 15675.61 i-amilol z, < User Modified Appendix 2 - 4 031141 in pairs of these fractions and gases dissolved in an alcohol-containing liquid. - 5 031141 L A v V £ 0 0 0 0 Ϊ 0 0 0 0 0 0 ‘0 BUT , _ t ...... 1 .............. U .D. 3 .. ,, I, <, 1 * Y External Standard Report Data File Name C: \ PROGRA ~ 1 \ BELHARD \ 1 \ DATA \ SIVUHA \ NV-Fa 9 6 9.D Operator Page Number one Instrument ANALYZERl Vial number Sample Name KGF of course Injection Number Run time ear code Sequence line Acquired on 02 Feb 10 01:21 PM Instrument Method SIVUHA.MTH Report Created on 02 Feb 10 02:05 PM Analysis Method SIVUHA.MTH Last Recalib on 02 Feb 10 08:38 AM Sample amount 0 Multiplier: one Istd amount Sample info Siq. 1 in C: \ PROGRA ~ l \ BELHARD \ l \ DATA \ SIVUHA \ NV ~ Fa969.D Ret time area Type Width Ref # mg / L Name ---one------------------ -------------one Nd 6.010 3874 BB 0.033 one 109.741 Acetaldehude 7.030 1017 BB 0.041 one 30.769 Methylacetate 7.994 45646 VB 0.053 one 1070.140 Ethylacetate 8.208 32384 BB 0.051 one 0.0981 Methanol 8.856 * not found * one i-propanol 12.536 415178 BB 0.076 one 6105.184 n-propanol 13.598 * not found * one Krotonaldehude 14.744 1516636 BB 0.088 one 17961.66 i-Butanol 17.140 4662 BB 0.076 one 58.364 n-Butanol 19.616 1277897 VB 0.097 one 13670.32 i-Amilol all < calibrated peaks were found Appendix 3