WO2009041929A1

WO2009041929A1 - Organic raw material extracting method and a plant for carrying out said method

Info

Publication number: WO2009041929A1
Application number: PCT/UA2008/000016
Authority: WO
Inventors: Lev Lutfullovich Telyashov; Aleksandr Viktorovich Bolmosov
Original assignee: Lev Lutfullovich Telyashov; Aleksandr Viktorovich Bolmosov
Priority date: 2007-09-24
Filing date: 2008-03-20
Publication date: 2009-04-02

Abstract

The invention relates to producing extracts which are valuable, environmentally sound and irreplaceable components for producing goods in the food, pharmaceutical, chemical, perfume, cosmetic and other industries which use natural substances, such as liposoluble vitamins, provitamins, biologically active agents and wax-lile compounds, taste- and aroma-carrying complexes, phytoncides and antioxidants. The inventive organic raw material extracting method consists in preparing a raw material and supplying it, together with a co-current additional extractant flow, and, after extraction and separation, respectively, in passing micelle and the extractant though filtering electrostatic barriers at the exit from an extractor and a separator. The inventive extracting plant comprises a disintegrator, a vessel with a raw material stirrer and a dosing unit for a cosolvent of solid raw material, the electrostatic barriers being disposed in the cavities upstream of the output pipes of the extractor and separator. The invention makes it possible to increase the selectivity, purity of a final product and to enhance the yield thereof.

Description

The method of extraction of organic raw materials and installation for extraction The invention relates to the production of extracts, mainly using carbon dioxide (CO ₂ ), which are valuable, environmentally friendly, irreplaceable components in the manufacture of products in the food, pharmaceutical, chemical, perfumery, cosmetics and other industries using natural substances such as fat-soluble vitamins, provitamins, biologically active substances and wax-like compounds, flavoring and aromatic Suitable complexes, volatile, antioxidants.

A known method for producing CO ₂ extracts described in the patent of the Russian Federation N ° 2041254, published 09.08.95, the IPC class CI lB 1/10. The method is implemented using the installation, which consists of an extractor, a micelle distiller — a separator, a condenser, and a receiver — a liquid carbon dioxide (CO ₂ ) storage device.

A method for producing CO ₂ extracts involves grinding the raw material, its flow-through extraction with carbon dioxide in the extractor at equilibrium pressure by repeated circulation, draining the micelle, followed by distillation and condensation of carbon dioxide. Moreover, before flow extraction, gaseous carbon dioxide is introduced into the lower part of the extractor until it reaches a pressure of at least 50% of the equilibrium pressure, and then liquid carbon dioxide is supplied from below until complete equilibrium pressure is reached. Common essential features of the method are grinding the raw material, its extraction with carbon dioxide in the extractor by repeated circulation, draining the micelle, followed by distillation and condensation of carbon dioxide. The disadvantages of this method are the low selectivity and performance due to the fact that a number of organic substances dissolve in liquid carbon dioxide at approximately the same, low speed and the circulation of the extractant occurs only due to convection. The latter circumstance leads to the need for cascading placement of installation elements in space, which makes it inconvenient in installation and operation. In addition, the operation of the installation is cyclical in nature, requiring a complete stop of the process, removing the mesh cup with meal, placing a new portion of raw materials in another mesh cup, purging the extractor and restoring the specified pressure and temperature parameters. A known method of extraction of raw materials described in the patent of the Russian Federation JSГ ° 2135551, published on 08.27.1999, IPC class Cl 1B1 / 10.

A method of extracting plant materials includes grinding the raw material, impregnating the raw material with a solvent. The grinding of raw materials is carried out to particles with a size of 0, 1 - 0.2 mm Impregnation of the raw material is carried out with stirring by a polar solvent in the ratio of raw materials to solvent 8: 1 - 40: 1, then the impregnated raw materials are extracted with a non-polar solvent, liquid carbon dioxide.

Common essential features is that the method of extraction of plant materials includes grinding the raw material, impregnating the raw material with a solvent. Impregnation of the raw material is carried out, with stirring, with a polar solvent. The disadvantages of this method are the low yield, selectivity and performance due to the fact that a number of organic substances dissolve in liquid carbon dioxide at approximately the same, low speed. The speed and depth of extraction is inversely proportional to the particle size of the feedstock, and in the known method it is possible to use grinding to a particle size of not less than 0.1 mm, which does not sufficiently increase the contact surface of the feedstock with the extractant, but further reduction in particle size is not possible, due to the occurrence of the process of harmful entrainment undissolved particles along with the extract. Low yield, selectivity and the purity of the final product — extract — is determined by the entrainment of insoluble small particles of liquid and solid raw materials from the extractors and the entrainment of the non-precipitated extract from the separators. Low productivity is additionally due to partial harmful entrainment of the extract. The closest is the method and installation for extraction at supercritical pressures, described in the book "Extraction of carbon dioxide in food technology", the authors Kosheva E. P., Blyagoz X P. Maykop: Maykop State Technologist, Institute, 2000, p. 316-322. In the method, to increase the selective solubility of substances, carbon dioxide (CO ₂ ) is used in a supercritical state, which allows fractionation — separation of raw materials of complex composition into components — by changing the temperature and pressure of the extractant. To perform the method, the plant material, which comes in bales or bales, is unpacked, loosened and cleaned on separators of metal impurities, stones and stems. The grinding of plant materials is carried out in an inert gas atmosphere. The feed is loaded into the extractor. Liquefied gas is pumped to a heat exchanger in which it is heated to 31.2 ° C. Being in a critical state, the solvent (extractant) passes through the feedstock and extracts the target components. After the extractor, the micelle passes through a pressure reducing valve, while the pressure decreases, the carbon dioxide partially evaporates.

In the separator - evaporator, the extract is heated and the residue of the solvent (extractant) is removed from it. It condenses (turns into a liquid state) in the condenser, enters the collector, and then again enters the extraction. The resulting extract from the separator - evaporator is fed to homogenization and conditioning.

The process is carried out in the device shown in Fig. 4.5. books. A liquid solvent (extractant) is discharged from the reservoir (cylinders with liquid CO ₂ ) in a state of subcritical pressure and subcritical temperature. The necessary subcritical temperature of carbon dioxide is set in the heat exchanger, and the required supercritical pressure is achieved by a high-pressure pump. Through the flow meter, carbon dioxide enters the extractor, where the extraction of the starting material. Is filled and the extractor is unloaded either with interruption, by opening and closing the top fitting after each extraction, or continuously, through the use of high-pressure gate locks, which without significant pressure reduction ensure a constant supply of fresh granules and unloading of extracted meal. The pressure of liquid carbon dioxide after exiting the extractor is determined by the pressure sensor. The micelle containing the extracted components of the hop is fed through a control valve and a heat exchanger to a pressure tank (separator), in which, when the pressure decreases, the extracted product, liquid and gaseous carbon dioxide, are simultaneously located. In a pressure tank (separator), hop extract precipitates and is discharged through a valve. Exiting the pressure tank (separator), carbon dioxide can be recycled through the pipeline. To control the pressure on the lines, pressure gauges are provided. Common essential features is that the extraction method includes counter vertical supply of raw materials and extractant, throttling and heating of the micelle obtained, separating the extract and condensing the gaseous extractant, increasing the pressure and temperature of the extractant to preset values and its reusable circulation.

The disadvantages of this method are the low speed, depth, selectivity of extraction. The speed and depth of extraction is inversely proportional to the particle size of the feedstock, and in a known installation it is possible to use grinding to a particle size of at least 1 mm, which does not sufficiently increase the contact surface of the feedstock with the extractant, but limits the entrainment of undissolved particles (meal) along with the extract. Low selection, selectivity and purity of the final product - extract are caused by harmful entrainment of insoluble small particles of liquid and solid raw materials from the extractors and also by harmful entrainment of non-precipitated extract from the separators. Low productivity is associated with the first two drawbacks, partial ablation of the extract from the separators, its useless circulation, as well as the lack of a quantitative criterion that determines the time of economically profitable end of the process, therefore, in known installations, they simply set the extraction time with a margin. The main the disadvantages of the prototype are a consequence of the technical contradiction that has not been eliminated in the prototype, which consists in the fact that the particle size of the raw materials must be very small at the same time — for quick and deep extraction and large — to eliminate harmful entrainment. The aim of the invention are to increase the yield and purity of the final product, increasing productivity.

The essential features of the method is that the method of extraction of organic raw materials includes counter vertical supply of raw materials and extractant, throttling and heating of the micelle obtained, separating the extract and condensing the gaseous extractant, increasing the pressure and temperature of the extractant to the specified values and its multiple circulation. The raw materials are prepared and fed with a satellite additional stream of extractant, and after extraction and separation, respectively, the micelle and extractant are passed at the outlet of the extractor and separator through filtering electrostatic barriers.

Grinding of solid raw materials to the degree of fine and ultrafine grinding is performed and a co-solvent is mixed with the liquid, and during the extraction of liquid raw materials, the co-solvent is introduced into the confluent and ascending counter flows of the extractant. The polarity of the electrostatic barrier in the extractor is set to the opposite micelle charge, and the polarity of the electrostatic barrier in the separator is set to the same polarity with the micelle, during the extraction process the dielectric constant and the tangent of the dielectric loss angle of the micelle with the extractant are measured, controlling the concentration and composition of the micelle, and after there is no decrease in concentration over the course of control time stop the extraction process. Carbon dioxide is used as an extractant.

Extraction is carried out in parallel in several extractors and separators, or alternately in several extractors and separators. Heating is performed by induction-free inertia electric heating. When extracting a non-polar fraction, the crushed raw material is mixed with a liquid with a co-solvent of non-polar nature, and during the extraction of a polar fractions of raw materials are mixed with a liquid cosolvent of polar nature.

Distinctive essential features valid in all cases is that the raw materials are prepared and fed with a satellite additional flow of extractant, and after extraction and separation, respectively, the micelle and extractant are passed at the outlet of the extractor and separator through filtering electrostatic barriers.

Distinctive essential features valid in some cases is that they grind solid raw materials to the degree of fine and ultrafine grinding and mix them with a liquid co-solvent, and during extraction of liquid raw materials the co-solvent is introduced into the satellite and upstream countercurrent flows of the extractant.

The polarity of the electrostatic barrier in the extractor is set to the opposite micelle charge, and the polarity of the electrostatic barrier in the separator is set to the same polarity with the micelle, during the extraction process the dielectric constant and the tangent of the dielectric loss angle of the micelle with the extractant are measured, controlling the concentration and composition of the micelle, and after there is no decrease in concentration over the course of control time stop the extraction process. Carbon dioxide is used as an extractant. The extraction is carried out in parallel in several extractors and separators or the extraction is performed alternately in several extractors and separators. Heating is performed by induction-free inertia electric heating. When extracting a non-polar fraction, the crushed raw materials are mixed with a liquid with a non-polar co-solvent, and during extraction of the polar fraction, the raw materials are mixed with a liquid with a co-solvent of a polar nature.

The implementation of the described method allows to increase the yield, purity of the final product and productivity, since the electrostatic barriers do not allow harmful entrainment of crushed raw materials and micelles, respectively, from extractors and separators, due to which it is possible to grind solid raw materials to sizes of 10-40 microns and in fewer cycles and less time provides a homogeneous product of high purity, with a high percentage of output. The choice of parallel or sequential extraction and separation, for specific types of raw materials, further increases the productivity and yield of the final product. There is no needless circulation, since the output of the extract from the raw material, which is processed, is controlled, and the circulation is completed at an economically feasible time.

A known installation for producing CO ₂ extracts is described in the patent of the Russian Federation JV ° 2232800 filed August 27, 2002, published in the Bulletin July 20, 2004, class MPC CPl / 10. The installation includes several extractors, an evaporator-condenser, a drive for solvent. In the installation, the extractors are connected by pipelines in a ring circuit with controlled valves, which ensure that the extractors are subsequently turned off sequentially for reset. A combined evaporator-condenser is located above the extractors, in which the annular space is a zone of evaporation of carbon dioxide from a micelle, and the tube space is a zone of condensation of carbon dioxide vapor. After the evaporator, a film final distiller is installed. The annular space of the evaporator-condenser is connected to the compressor inlet of the turboexpander-compressor unit, the output of the compressor of the unit is connected to the input of the second stage compressor, the output of which is connected to the tube space of the evaporator-condenser. The outlet of the evaporator-condenser tube space is connected to the inlet of the turbo-expander of the turbo-expander-compressor unit, which makes it possible to use the energy of the condensate under increased pressure to compress carbon dioxide vapor. The output of the turboexpander and the steam space of the final distiller are connected to the inputs of the mixing condenser, the output of which is connected to the solvent collector.

Common essential features are that the installation includes several extractors, a condenser, a solvent reservoir, and extractors are connected by pipelines controlled by valves.

The disadvantages of the known device are the low extraction rate, low yield of the finished product and insufficient extraction selectivity. The extraction rate and the yield of the finished product are inversely proportional to the particle size of the raw material, and in this installation, grinding dimensions of 0.1-0.2 mm, as described in the patent of the Russian Federation JCH ° 2135551 of the same applicant. The low selection, selectivity and purity of the final product-extract are due to the entrainment of insoluble small particles of liquid and solid raw materials from the extractors and the entrainment of the non-precipitated soaking extract from the separators. In addition, the installation is distinguished by low productivity associated with the first two drawbacks, partial ablation of the extract from the separators, its useless circulation, and the absence of a quantitative criterion that records the end of the process. Usually just set the extraction time with a large margin, which leads to unnecessary extraction cycles. The closest installation for supercritical extraction is the installation described in the patent of the Russian Federation N ° 2292385, published on 01/27/2007, class IPC B01D11 / 02. Installation for the supercritical extraction process, contains a pump and a high-pressure cylinder, an extractor, a separator, a storage tank for solvent, connecting pipelines, measuring and shut-off and control valves. The installation additionally contains a system for cleaning the solvent from impurities, a system for its regeneration, a group of sequentially installed separators for fractionation of the target product and an automatic system for measuring and controlling the thermodynamic parameters of the solvent in the extractor and separators to maintain them in a given pressure and temperature range.

The installation comprises at least one additional high-pressure cylinder mounted parallel to the main high-pressure cylinder with the possibility of alternating or simultaneous operation. The automatic system for measuring and controlling the thermodynamic parameters of the solvent and the units of the installation are capable of carrying out an extraction process in it at a temperature from plus 20 ° С to plus 600 ° C and a pressure from 0 to 60 MPa, followed by fractional separation of the target product at a temperature from minus 5 ° C to plus 20 ° C and pressure from ODMPa to 0.5 MPa.

Common essential features is that the extraction plant contains at least one pump, extractor, separator, condenser, storage tank for extractant, connecting pipelines, measuring and shut-off and control valves, automatic system measuring and controlling thermodynamic parameters in the extractor and separator.

The disadvantages of the installation are low selectivity and purity, low yield of the finished product and low productivity due to the fact that a number of organic substances dissolve in liquid carbon dioxide at approximately the same, low speed. The design of the device does not exclude the harmful entrainment of crushed raw materials from extractors and separators, its unnecessary circulation, and there is no quantitative criterion for registering the economically feasible end of the process. Usually just set the extraction time with a margin.

The aim of the invention is to increase the selectivity, purity of the final product, increase the yield of the product, and accordingly productivity, the exclusion of unnecessary circulation.

The essential features of the invention is that the extraction plant contains at least one pump, extractor, separator, condenser, storage tank for the extractant, connecting pipelines, measuring and shut-off and control valves, an automatic system for measuring and controlling thermodynamic parameters in the extractor and separator. The installation additionally contains a solid raw material disintegrator, a container with a raw material mixer and a solid raw material co-solvent dispenser, dispersant mixers that are connected to the raw material inlets to the extractors, electrostatic barriers are installed in the cavities in front of the outlet pipelines from the extractor and separator, induction windings are placed on the extractor and separator housings heating, and the automatic system for measuring and controlling thermodynamic parameters is supplemented by a micelle concentration sensor.

Electrostatic barriers are made in the form of metal grids installed in insulating glasses, which are fixed on the inner surfaces of the extractor and separator, metal grids are connected by insulated electrodes to a source of high constant voltage.

Inputs of pipelines of raw materials and micelles are located below the level of grids electrostatic barriers in the cases of the extractor and separator and are equipped with downward curved tubes, and the pipeline for supplying the extractant to the extractors branches into a pipeline connected to the disperser-mixer and the pipeline connected to the extractor through a throttle. Distinctive essential features valid in all cases is that the installation additionally contains a solid raw material disintegrator, a container with a raw material mixer and a solid raw material co-solvent dispenser, a disperser-mixer, which is connected to the raw material input to the extractor, in the cavities in front of the outlet pipelines from the extractor and separator are installed electrostatic barriers; induction heating windings are placed on the extractor and separator bodies; moreover, an automatic system for measuring and controlling thermo ynamic parameters supplemented sensor micelle concentration.

Distinctive essential features, valid in some cases, is that the electrostatic barriers are made in the form of metal grids installed in insulating cups, which are fixed on the inner surfaces of the extractor and separator, metal grids are connected by insulated electrodes to a source of high constant voltage. Raw material and micelle pipelines inlets are located below the level of electrostatic barrier grids in the extractor and separator housings, and are equipped with downward curved tubes, and the extractant supply pipeline to the extractors branches into a pipeline connected to the dispersant - mixer and the pipeline connected to the extractor through a throttle. The presented installation allows you to increase the selectivity and purity of the final product, since the electrostatic barriers do not allow harmful entrainment of the crushed raw materials and micelles from extractors and separators, respectively, the productivity and yield of the final product are increased, since the grinding of raw materials is allowed and performed to sizes of 10-40 microns, and unnecessary circulation is excluded, since micelle concentration is controlled. The figure 1 shows a diagram of an installation for extraction.

The installation consists of the main components: a doser for a co-solvent of solid raw materials 1, a container 2 with an agitator for liquid or ground solid solvents, extractors 3 and 4, separators 5 and 6, the first

5 of a heating heat exchanger 7, a condenser 8 connected to a refrigerating machine 9, a high pressure pump 10 for supplying carbon dioxide, a high pressure pump 11 for supplying a co-solvent, a high pressure pump 12 for supplying raw materials, a vessel with a co-solvent 13 and a second heating heat exchanger 14. Extractors 3, 4 are equipped with dispersant mixers 15 and 16, windings

10 17 for inertialess inductive heating and insulated electrodes 18 connected inside the extractors with metal grids 19, which are insulated from the extractor bodies by dielectric cups 20. Separators 5 and 6, similarly, are equipped with windings 21 of inertialess induction heaters, electrodes 22, metal grids 23 s

15 with a mesh size of 1 to 3 mm, dielectric glasses 24 and micelle input tubes 25. The electrodes 18 and 22 are connected to a two-channel source of constant high voltage 26. The installation is equipped with remotely controlled shut-off valves 28-40, relief valves 41-45 and valve 55, check valves 46 and 47. Before the first heating heat exchanger 7, a concentration sensor is cut into the common pipe 7 into 0 48, for example, of a capacitive type, and an adjustable choke 49, which, in order to prevent freezing, are located in the immediate vicinity of the heat exchanger 7. Chokes 50 and 51 with chokes are placed in front of the lower entrances to the extractors 3 and 4 with my washers. A second concentration sensor 52 is installed in the common pipeline at the outlet of separators 5 and 6. In the diagram, disperser-mixers 15, 16 are located outside the extractors 3 and 4 and are connected by curved guide tubes 53 to the cavities of the latter, but they can be placed coaxially inside the extractors. Unlike extractors 3 and 4, separators 5 and 6, the tank 2 is not designed for high pressure, has a small wall thickness and sufficiently high heat conductivity, therefore its heater is made in the form of a jacket 54 for the passage of a liquid coolant. The extractant accumulator 56 serves as a carbon dioxide receiver. Disintegrator 57 is connected to dispenser 1. Pipelines 58 and 59 are connected through valves 29 and 32 to dispersers - mixers 15 and 16, and pipelines 60 and 61, through valves 30 and 35 and through inductors with throttle washers 50 and 51 are connected to extractors 3 and 4.

The proposed method for the extraction of organic raw materials in the installation according to the invention is as follows. The solid raw materials are crushed in a disintegrator 57 to a particle size of tens of microns, that is, to a level of ultrafine grinding, and through dispenser 1 it is fed with a co-solvent, non-polar liquid, having maximum solubility in carbon dioxide at lower temperatures and pressures than those recovered extracts into a container 2 and mix. So in preparation for the extraction of lecithin from egg powder, refined vegetable oil can be used as such a liquid. Fluid feed, for example a phospholipid concentrate, is not mixed with the cosolvent at this stage. The resulting fluid mixture is heated and stirred in a container 2. After purging the system with carbon dioxide gas with closed valves 41, 42, 43, 44.45 and all valves except valve 30, the chiller 9, pump 10 are turned on and supplied, not shown in the heater diagram, hot water to heat exchangers 7, 14, as well as power to the windings 17, performs fast inertialess induction heating. As a result of these operations, the temperature of the case of the extractor 3, as a secondary short-circuited winding of the transformer, rises to the calculated value of the dissolution temperature of the first component, for example, fats (oils). The temperature of carbon dioxide in extractor 3 is also brought to the calculated value, and the pressure is 2-2.5 MPa higher than the calculated one, while the extractant itself goes into a supercritical (fluid) state. Following this, the shut-off valves 28, 29, 36, 37, 55 are opened, the pump 12 is turned on to supply raw materials from the tank 2 and the high voltage source 26, and the opposite is applied to the electrodes 18 of the extractors 3 and 4 and the electrodes 22 of the separators 5 and 6 the sign is a high-voltage constant voltage of 30-40 kV. As soon as carbon dioxide begins to circulate on the ring 3, 33, 48, 49, 7, 36, 25, 5, 37, 52, 8, 56, 10, 14, 30, 50, 3 and branch 29, 15, 53, 3 the pressure in the extractor drops due to the restrictor 50 to the calculated values and the raw materials supplied under more high pressure, interacting with carbon dioxide in the mixer-dispersant 15 is injected into the extractor 3. The torch of the mixture injected from the guide tube 53 from top to bottom collides with a stream of fluid supplied from below to the extractor 3. As a result of intense turbulence of the flows

5 and a large area of contact of carbon dioxide with particles (drops) of raw materials, an accelerated deep dissolution of the first component, fats (oil), occurs with the formation of a micelle. The micelle has a charge in sign opposite to the charge of the grid 19, therefore it is accelerated by the potential of the grid and freely passes to the separator 5 along the above path through an adjustable choke

10 49, at the outlet of which the micelle pressure is reduced to 5-7 MPa, and the temperature is 20-30 ° C. In the heat exchanger 7, the micelle is heated to the temperature of the boundary state of the carbon dioxide liquid-gas. For example, at a pressure of 6 MPa, the boundary temperature is 21 ° C. Next, the micelle is thrown through the tube 25 into the cavity of the separator 5 heated by means of windings 21 induction

15 heater to a temperature of more than 25 ° C. Carbon dioxide instantly goes into a gaseous state and disappears, passing through a grid 23, a valve 37, a sensor 52 that monitors the purity of gaseous carbon dioxide and enters a condenser 8, in which it is cooled to 10-15 ° C and goes into a liquid state. Liquid carbon dioxide is collected in the extractant storage tank

20 56, from where it enters the high-pressure pump 10, which raises the pressure 2-2.5 MPa higher than the calculated one, and then heats up in the heat exchanger 14 to a temperature slightly higher than the calculated one, by the magnitude of the temperature drop due to the throttling of carbon dioxide by a 50 throttle with a throttle washer. Soaking extract particles in separator 4 and entrained

25 ascending flows of carbon dioxide can not pass the grid 23, as they have the same charge with it. The purity of the circulating carbon dioxide is controlled by a concentration sensor 52, the zero mark of which is the value of the electric capacity of the sensor, filled only with carbon dioxide gas under operating pressure. During the first stage of extraction

30 there is a repeated circulation of carbon dioxide with the supply of raw materials from the tank 2, the accumulation of fat-free raw materials in the extractor 3 and fats (oils) in the separator 5. The conditions for the end of this stage is the filling of the lower third .

14 of the extractor 3 with nonfat raw materials and stopping the drop in micelle concentration during the control time, for example 1 minute recorded by the concentration sensor 48, the zero mark of which is the electric capacitance of the sensor filled with carbon dioxide in a supercritical operating state.

The second stage consists in extracting the second component, for example, lecithin, from nonfat raw materials and preparing the extractor 4 for the first stage. The valves 55, 28, 36, 37 are closed, the valves 35, 38, 39 are opened, the polarity of the high-voltage voltage source 26 is reversed, the walls of the extractor 3 are heated to a higher temperature corresponding to the maximum dissolution rate of the second lecithin component, and the extractor 4 is heated to extraction temperature of the first component (fats). At the same time, the pressure at the outlet of the pump 10 is raised to a pressure value exceeding the calculated value for the second component 2-2.5 MPa higher than the calculated one. After reaching the pressure in the extractor 4 of the calculated value for the first component, close the valve 35, open the valve 40 and turn on the pump 11. Polar cosolvent - ethanol is mixed with carbon dioxide in a concentration of 10-15%. Thus obtained eluent flows from below to the extractor 3 and maintains the skimmed raw materials in a fluidized state, and the stream passing through the guide tube 53 makes it turbulent. The micelle formed as a result of the dissolution of lecithin has an opposite charge compared to the fat micelle, therefore, after changing the polarity on the grid 19, the lecithin micelle freely passes the electrostatic barrier and enters the separator 6 along the already known path. Thus, fats are collected in the separator 5 (oil ), which can be dumped into the appropriate collection by briefly opening the valve 44 until the end of the second stage - lecithin extraction. After extracting lecithin in a cost-effective concentration from nonfat raw materials, close valves 29, 30, 33, 38, 39, 40, open valves 55, 31, 32, 34, 35, 36, 37, turn on pump 12 and turn off pump 11. Pump 10 rebuild on the 1st extraction mode - with less feed pressure. Then open for a short time the relief valve 42 and from the extractor 3 with compressed dioxide carbon residues are thrown away. Next, the extractor 3 is prepared as described above for the next extraction of the first component (fats) from raw materials.

Thus, an almost continuous extraction of two extracts is realized. In general, extraction with a large number of extracts is possible. In this case, the same number of separators is required.

A circuit with parallel operation of extractors has a higher productivity. Given that the extraction process takes from 0.5 to 3 hours, a break for discharge of extracts and waste within 1-2 minutes practically does not reduce the productivity of the installation. It is possible to recommend for a short extraction process the circuit of alternating inclusion described in detail above, and for a long process - a parallel one. If it is necessary to increase productivity with a short extraction process, a mixed scheme is recommended - alternating operation of parallel connected extractors. During the setup process, the extraction of organic raw materials was carried out using the invention, while checking the efficiency of the electrostatic barrier, the power supply of the electrostatic barrier was turned off, and insoluble small particles of raw materials were removed from the extractors, not settled extract was taken from the separators, and it was impossible to ensure the purity of the final product.

We give examples related to methods for producing lecithin.

Example 1. Extraction of a single component. At the inventive installation, soybeans are loaded into a disintegrator, for example, a finger mill, and then they are dispensed in the form of a powder with a particle size of 40 + 10 μm in a ratio of 1: 5-1: 2 with a co-solvent, in particular ethyl alcohol (ethanol), into a container with a stirrer. In this tank, as a result of mixing and heating to a design temperature of 80 ° C, a fluid mixture forms, which is fed to the disperser-mixer of the first extractor by a high-pressure pump. Carbon dioxide fluid is supplied to the same dispersant-mixer, as a result of which a dispersed system is formed at the outlet of the dispersant, soybean powder is an eluent (a mixture of carbon dioxide and ethanol). The downward dispersed dispersed system collides with an upward heated 80 ° C with a stream of carbon dioxide. In the lower part of the extractor, mixing and turbulization of the flows and a decrease in the concentration of ethanol in carbon dioxide occur to a calculated value in the range from 12% to 15%. The pressure in the extractor also decreases to a calculated value in the range from 32 MPa to 36 MPa. Ethanol plays the role of a polar cosolvent, providing the formation of a lecithin micelle, the flow of which goes around the torch of the dispersed system and is accelerated in the field of the electrostatic barrier network, which is under the “negative” potential. Partially dissolved “fats” having a “negative” charge, which is opposite to the charge of lecithin micelles, are discarded by the field of the electrostatic barrier. Thus, a high selectivity of extraction is achieved. Then a micelle with unreacted carbon dioxide enters the concentration sensor, which is a capacitive sensor connected to a measuring bridge calibrated as a percentage of the micelle concentration in carbon dioxide, and then to an adjustable inductor and heater. At their outlet, the pressure drops to 6-7 MPa, and the temperature drops to 20-27 ° C, that is, to the parameters of the metastable state of carbon dioxide. The mixture is thrown into the separator, the temperature of which is maintained higher than that of the mixture by 5 ° C. Additional heating of the mixture leads to the transition of carbon dioxide into a gaseous state and the precipitation of lecithin with ethanol. The entrainment of lecithin particles from the separator at high carbon dioxide circulation rates is prevented by the electrostatic barrier of the same potential as lecithin. The purity of carbon dioxide after the separators is controlled by a second concentration sensor, which is also a capacitive sensor connected to the measuring bridge. During the operation of the installation, an oily meal in the form of a fluidized bed accumulates in the lower part of the extractor due to turbulent flows. An increase in its volume is permissible until it becomes a hindrance to extraction, which will affect the decrease in micelle concentration. After that, the process is switched to the second extractor, and the first is cut off by closing the valves on the inlet and outlet lines. Then open the discharge valve, loose meal under high pressure is ejected from the extractor into the receiving tank. The discharge valve is closed and the set pressure and temperature are restored in the extractor. Example 2. Extraction of a single component. Dry egg yolk granules are loaded into the plant's disintegrator, which is then fed into a container with a mixer in the form of ultrafine powder through a batcher. Further, everything happens as in example 1. At the same time, oil protein, also valuable, is unloaded from the extractors.

5 food and pharmaceutical product.

Example 3. Extraction of two components of fat (oil) and lecithin. A phosphatide concentrate (oil and fat waste), which is a viscous liquid under normal conditions, is loaded into a container with a stirrer. In a tank, it is heated to an oil extraction temperature from

10 60 ° C to 70 ° C, after which a high pressure pump is fed into the dispersant. Carbon dioxide fluid is supplied there at the same temperature. From below, an eluent is fed into the extractor in the form of carbon dioxide fluid and 7% ethanol, which interferes with the stream of dispersed dispersed system phosphatide concentrate-carbon dioxide fluid. Dispersion of the dispersed system is carried out

15 at a rate exceeding the amount of eluent required for extraction with a single circulation of carbon dioxide. Thanks to this, the formation of a high-speed torch is possible. The dose of the phosphatide concentrate is set from the conditions for the existence of a fluidized bed in the lower third of the length of the extractor. The pressure is set in the extractor from 27 MPa to 30 MPa,

20 which, along with a temperature in the range from 60 ° C to

70 ° C optimal parameters for the extraction of oil, which settles in the first separator. After the concentration sensor detects the cessation of the drop in micelle concentration within 2 minutes, the first extractor is cut off by closing the valves, and the second extractor with the second

25 dispersant mixer. After the extraction of oil in the second extractor is completed, it is also cut off and the first extractor is turned on, in which the process of lecithin extraction from the residues of defatted phosphatide concentrate (after the first stage of the process) is carried out at higher parameters of carbon dioxide, pressure from 32 MPa to 36 MPa and temperature

30 80 ⁰ C. Moreover, the proportion of ethanol in the eluent supplied from below to the extractor is from 12% to 15%. Lecithin settles with ethanol in another separator. After the extraction of lecithin in the first extractor, the same extraction produced in the second extractor, and unnecessary waste is discarded from the first.

Thus, the installation can be implemented in two modes of supply of raw materials: low-speed, when immediately (synchronously) extraction occurs and pulsed dosed feed. Alternate pulsed supply of a disperse system from dispersant-mixers of the first, second or more extractors with circulation of carbon dioxide through open extractors (parallel-series connection) and separators.

The proposed method and device allows not less than two times to increase the productivity of the extraction process of raw materials due to the permissibility of fine grinding, which increases the contact area of the raw material with the extractant, since the presence of an electrostatic barrier allows for high-quality fractionation of such raw materials. The selectivity and purity of the obtained extracts are above 99%.

Claims

Formula

1. The method of extraction of organic raw materials, including counter vertical supply of raw materials and extractant, throttling and heating the micelle obtained, separating the extract and condensing the gaseous extractant, increasing the pressure and temperature of the extractant to preset values and its reusable circulation, characterized in that the raw material is prepared and served with additional satellite extractant stream, and after extraction and separation, respectively, the micelle and extractant are passed at the outlet of the extractor and separator through fil truyuschie electrostatic barriers.

2. The method according to claim 1, characterized in that the grinding of solid raw materials to the degree of fine and ultrafine grinding is performed and mixed with a liquid with a co-solvent.

3. The method according to claim 1, characterized in that during the extraction of the liquid feed, the cosolvent is introduced into the confluent and upstream countercurrent flows of the extractant.

4. The method according to claim 1, characterized in that the polarity of the electrostatic barrier in the extractor is set to the opposite micelle charge, and the polarity of the electrostatic barrier in the separator is set to the same polarity with the micelle, the dielectric constant and the tangent of the dielectric loss angle of the micelle with the extractant are measured in the process of control the concentration and composition of the micelle, and after the absence of a decrease in concentration during the control time, the extraction process is stopped.

5. The method according to claim 1, characterized in that carbon dioxide is used as the extractant.

6. The method according to claim 1, characterized in that the extraction is carried out in parallel in several extractors and separators.

7. The method according to claim 1, characterized in that the extraction is performed alternately in several extractors and separators.

8. The method according to claim 1, characterized in that the heating is performed by induction without inertia electric heating.

9. The method according to claim 1, characterized in that when the non-polar fraction is extracted, the crushed raw materials are mixed with a liquid with a non-polar co-solvent.

10. The method according to p. 1, characterized in that during the extraction of the polar fraction, the raw material is mixed with a liquid co-solvent of a polar nature.

11. Installation for extraction, which contains at least one pump, extractor, separator, condenser, storage tank for extractant, connecting pipelines, measuring and shut-off and control valves, automatic system for measuring and controlling thermodynamic parameters in the extractor and separator, characterized in that additionally contains a solid raw materials disintegrator, a container with a raw material mixer and a solid raw material co-solvent dispenser, a dispersant-mixer, which is connected to the input of raw materials into the extractor, Electrostatic barriers are installed in the cavities in front of the outlet pipelines from the extractor and separator; induction heating windings are placed on the extractor and separator bodies; moreover, the automatic system for measuring and controlling thermodynamic parameters is supplemented by a micelle concentration sensor.

12. Installation according to claim 1, characterized in that the electrostatic barriers are made in the form of metal grids installed in insulating cups that are mounted on the inner surfaces of the extractor and the separator, metal grids are connected by insulated electrodes to a source of high constant voltage.

13. Installation according to claim 1, characterized in that the inputs of the pipelines of raw materials and micelles are located below the level of the networks of electrostatic barriers in the housings of the extractor and separator, and are equipped with downward curved tubes, and the pipeline for supplying the extractant to the extractors branches into a pipeline connected to the dispersant - mixer and piping connected to the extractor through a throttle.