RU2799374C2 - Installation for extraction of biologically active substances from vapour-permeable plant raw material - Google Patents

Abstract

FIELD: extraction technologies.

SUBSTANCE: invention relates to a plant for the extraction of biologically active substances from a vapour-permeable plant material. A universal extraction apparatus operating in mild extraction modes is designed to extract biologically active substances with pronounced physiological activity.

EFFECT: whole complex of the technological process takes place in one vat apparatus designed for extraction using vacuum, convective diffusion for extraction of biologically active substances from vapour-permeable plant materials.

2 cl, 1 tbl, 4 dwg

Description

Links

[1] Guidelines MP 2.3.1.1915-04 "Recommended levels of consumption of food and biologically active substances" (approved by the Federal Service for Supervision of Consumer Rights Protection and Human Welfare on July 2, 2004).

[2] Patent RU 2213606, B01D 11/02.

Technical field

The invention relates to the technology of extraction using vacuum, using convective diffusion, during the extraction of vapor-permeable plant materials, and can be used to extract valuable biologically active components (substances) according to the text of biologically active substances used in various industries. An important feature of the extraction of biologically active substances from a vapor-permeable raw material is that its physical properties change significantly, the transfer of extracting substances due to the heterogeneity of the concentration field (mass transfer) can be carried out by convective diffusion, while the extraction rate, determined by the driving force of the process (the difference in concentrations of the extractable substances in the liquid filling the pores of the raw material, and in the bulk of the solvent in contact with the surface of the solid particles) and diffusion resistance at each stage.

Extraction of biologically active substances from wild-growing vapor-permeable raw materials depends on many factors, the most important of which are temperature, the degree of grinding of raw materials, the choice of extractant, the ratio of raw materials and solvent (hydromodulus) and the duration of extraction; penetration of the extract into the pores of the raw material; dissolution of biologically active substances in the extract; transfer of the extractable from the depth of the solid particle to the interface; for fresh raw materials with the help of mass conduction, since the mechanism is complicated by swelling; transfer of biologically active substances from the interface into the depth of the extract using convective diffusion (mass transfer). Also, there are factors that determine the cost-effectiveness and efficiency of the installation (apparatus), such as evaporation and concentration of the final product, as well as complete recirculation of the main solvent, that is, the installation (apparatus) should have the simplest and most understandable way of working, while not using no mechanical means when mixing incoming raw materials, moving raw materials from one extractor (reactor) to another, using other mechanisms or units. The installation (apparatus) must have a working capacity (for processing the loaded raw materials in kg of dry matter) from 200 kg to 2000 kg of processed incoming raw materials. The installation (apparatus) can be used for medium and small laboratories, as well as for medium-sized industries involved in the study and implementation of the extraction (extraction) of biologically active substances into a practical and commercial field of activity.

That is, if you pour the feedstock into the reactor-extractor, all the processes of extraction, evaporation, concentration, recirculation of the main solvent and drying of the input raw materials should occur in one vat apparatus.

State of the art

The installation (apparatus) is designed for extraction (recovery) of biologically active hydrophilic substances (substance that tends to be wetted by water) under vacuum with a solvent content of 40-70% while maintaining a temperature regime of 30-40 ° C, and hydrophobic substances (a substance that cannot be wetted by water) from vapor-permeable plant materials, which include wood chips, knots, stems, bark, rhizomes, shoots, leaves, seeds, cones, and others. Biologically active substances (BAS) - the general name of substances that have a pronounced physiological activity, combines substances that have a noticeable stimulating or inhibitory effect on biochemical processes in vivo or in vitro, including in accordance with the classification of Methodological recommendations MP 2.3.1.1915-04 ("Recommended levels of consumption of food and biologically active substances") [1], namely:

- various groups of flavanoids (flavanols and their glycosides - quercetin, kemferol, rutin, etc.; flavones - luteolin, apigenin, etc.; flavonones - naringenin, hesperidin, etc.; dihydroflavanols (dihydroquercetin), proatocyanidins, catechins, anthocyanins, flavolignans - silybin, silidianin, silichristin, etc., isoflavones - genistein, daidzein, glycitein or isoflavone glycosides - genistin, daidzin, glycitin, anthraquinones - aloe-emodin, rapontin, rhein, fiscion, chrysophaco acid, sennosides A and B and others);

- phenolic compounds and simple phenols (hydroquinone, arbutin, hydroxycinnamic acids, etc.);

- polymeric phenolic (tannins, stilbenes);

- phenolic acids (hydroxycinnamic, acids (chicory, caftaric, chlorogenic, ferulic, caffeic, gallic, p-hydroxybenzoic)

- organic acids (angelic, succinic, malic, hydroxycitric, tartaric, glycolic, glyoxalic, isocitric, cinnamic, p-coumaric, valeric acid, etc.);

- sterols (beta-sitosterols, beta-sitosterol-D-glycoside, stigmasterol);

- betaine, betulin, hydroxycitric acid, gingosides, hypericin, glycyrrhizic acid, L-glutamine, curcumin, serotonin, schisandrin, theobromine, theophylline);

- forskolin (citrulline, eleutherosides);

- polysaccharides (galacto-glucomannans, polyfructosans, arabinogalactan, galactooligosaccharides, fructooligosaccharides, chitosan);

- dietary fibers (Pectin, gums, carrageenans, agar-agar, gum arabic), including insoluble ones (Cellulose, hemicellulose, lignin)

Deficiency of these nutrients and biologically active components in the diet leads to a decrease in the body's resistance to adverse environmental factors (maladaptation), the formation of immunodeficiency states, dysfunction of antioxidant defense systems, chronic diseases, an increased risk of developing common diseases, a decrease in the quality of life and the effectiveness of therapeutic measures. .

A device described in the patent (RU 2213606, B01D 11/02) is known, which implements this extraction method and is taken as a prototype for the proposed device, containing an extractant tank and an extractor connected by a pipeline through quick-acting valves to each other, with a condensate collector and a receiver, a vacuum a pump connected to the receiver, a reflux condenser is installed above the extractor, which ensures the condensation of extractant vapors, a heater and a pump, which provide heating and supply of heating fluid to the jacket of the extractant and extractor containers.

An important feature of the proposed installation is the use of "hot" steam, i.e. water vapor supplied directly to the extractor and mixed with vapor-permeable raw materials, which significantly speeds up the maceration process and allows substances to be extracted from the solution with one portion of the solvent, in addition, more efficient degassing of the raw materials occurs. The use of "hot" steam ensures the penetration of the extract into the pores of the raw material more efficiently; dissolution of biologically active substances in the extract; transfer of the extractable from the depth of the solid particle to the interface.

An important feature of the installation is the possibility of using convective heat transfer (convective diffusion) to carry out the process of heat propagation in a liquid from the surface of a solid body or to its surface simultaneously by convection and thermal conductivity, thus heat is distributed i.e. heat transfer by contact .. During heat transfer, heat propagates from the surface of a solid to a liquid through the boundary layer due to thermal conductivity and from the boundary layer to the liquid mass mainly by convection.

Also, an important feature of the installation is the possibility of using circulation-type extraction - a circulation extraction method based on the circulation of the extractant and the effective provision of the extraction rate determined by the driving force of the process (the difference in the concentration of the extractable substance in the liquid that fills the pores of the raw material, and in the bulk of the solvent in contact with the surface of solid particles) and diffusion resistance at each stage.

The inventive installation is novel in comparison with the prototypes, differing from them in such essential features as the presence of an extractor, a cube-collector of alcohol-soluble biologically active substances; cube-collector of alcohol-insoluble biologically active substances; alcohol receiver; refrigerator; dephlegmator; refrigerant supply systems.

The basis of the proposed installation was the already created pilot plant with the ability to load 1000 kg of dry raw materials, which is currently successfully operating, specializing to a greater extent in the extraction of polyphenol - dihydroquercetin and polysaccharide - larch arabinogalactan from larch chips. Both products have passed successful laboratory and pre-clinical trials in the USA, Europe, and are in commercial demand.

Disclosure of invention

The objective of the present invention is to develop a device that makes it possible to increase the operational capabilities of the extraction process by creating conditions for the extraction of various types of biological raw materials using a minimum amount of extractant and at the same time increasing the intensity of the process, the yield of extractable biologically active substances, and improving their quality.

To solve the problem, the installation includes processing raw materials with steam, extracting biologically active substances from vapor-permeable vegetable raw materials, drying crushed fractions of vegetable raw materials in one device, which includes an extractor with two cubes located under it - BAS collectors and a reflux condenser located above them. Application of convective heat transfer (convective diffusion). Implementation of heating of the extractant, extraction of raw materials at temperature conditions that do not cause denaturation of the material and extractable components (BAS) of raw materials. Provides for the use of a water-alcohol solution with an alcohol concentration of at least 20%, with an extraction module (extractant: raw material) of no more than 2.

During extraction, the alcohol in the BAS collection cube is heated with hot water supplied to the coil. The process is carried out under vacuum. Alcohol evaporates, alcohol vapors pass through the crushed fractions of raw materials and condense on a reflux condenser, flow down through the crushed fractions, extracting BAS. BAS remains in the collection, alcohol cycles several more times. When extracting BAS insoluble in alcohol, the water in the BAS collection cube is heated with hot water supplied to the coil. The process is also carried out under vacuum. Water evaporates, water vapor passes through the crushed fractions of the raw material and condenses on the reflux condenser, flows down the fractions, extracting BAS insoluble in alcohol. BAS remains in the collection, the water cycles several more times. When changing the solvent from alcohol to water, evacuation is carried out through a refrigerator, in which alcohol is condensed and returned to the technological process.

After obtaining an aqueous concentrate of BAS insoluble in alcohol, the process of drying sawdust is carried out by passing hot air through them for 4 hours. At the end of the drying process, with the help of a pneumatic suction, the reactor is cleaned from the crushed fractions of the raw material. The reactor is ready for the next load.

Brief description of the drawings

The functional diagram of the installation is shown in figure 1.

List of images with brief explanations:

The stages of the extraction process using the example of extracting dihydroquercetin (DHA) (an alcohol-soluble BAS) and larch arabinogalactan (AG) (an alcohol-insoluble BAS) from larch chips are shown in figure 2.

List of elements with brief explanations:

The operation of the reactors in a closed cycle is shown in figure 3.

List of elements with brief explanations:

The installation includes the following technological modules - figure 1:

5 extractor;

1 cube collection of alcohol-soluble biologically active substances;

3 cube collection of alcohol-insoluble (alcohol-insoluble) biologically active substances;

8 alcohol receiver;

7 refrigerator;

6 dephlegmator;

51 refrigerant supply systems.

Implementation of the invention

Extractor

The extractor is a column apparatus made of stainless steel. It has valves for evacuation and atmospheric pressure supply. The extractor is equipped with four temperature sensors to measure and display the temperature at different height points of the column and a vacuum gauge to control the pressure inside the column.

Compilation cubes

Cubes-collectors of alcohol-soluble and alcohol-insoluble biologically active substances are accumulative containers of liquid media, each with tubular heat exchangers. Cubes-collectors have valves for sampling, valves for evacuation and supply of atmospheric pressure. Each cube is equipped with float indicators of the liquid level and pressure and vacuum meters, as well as temperature sensors. Collecting cubes are connected to the extractor with flexible reinforced PVC hoses and stainless steel pipelines, which provide pumping of solutions from cubes to the extractor and back by switching the positions of the corresponding valves.

Alcohol receiver

The alcohol receiver is a storage container made of stainless steel. From the extractor, ethanol (alcohol) vapors condensed in the refrigerator enter the alcohol receiver. The alcohol receiver is equipped with a float indicator of the liquid level and a pressure and vacuum gauge, and also has a valve for sampling and valves for draining ethanol into external containers and into collection cubes of alcohol-soluble and alcohol-insoluble biologically active substances.

Dephlegmator

The reflux condenser is a system of tubular heat exchangers located in the upper part of the extractor and is designed to condense ethanol vapors. The refrigerant supply to the dephlegmator is carried out through an appropriate system (for each heat exchanger separately).

Fridge

The refrigerator is designed to condense ethanol and then drain it into the alcohol receiver. The refrigerator is connected to an extractor and a reflux condenser. It has a refrigerant supply through an appropriate system and a drain system. Through the refrigerator, the system is evacuated and atmospheric pressure is supplied.

Refrigerant supply system

It is a connection of the cold water supply system of the workshop with a refrigerator and a dephlegmator using valves that provide a coolant supply to each dephlegmator heat exchanger. Site effluents (washing water and refrigerant) are included in the plant's circulating water supply system.

Obtaining biologically active substances from plant materials is a complex process, which is a sequence of technological operations for the preparation of raw materials, extraction and subsequent separation of biologically active substances from the pulp and their purification to obtain final production products. The unit allows to carry out the operations of extraction of biologically active substances and regeneration of extractants in order to ensure their return to the production process. The stages of the extraction process are shown in figure 2, the timing diagram of the process is shown in table 1.

In the technological process of extraction, the following main stages and operations can be distinguished:

a) loading of raw materials and steaming;

b) extraction with ethanol:

- alcohol extraction;

- alcohol washing;

c) ethanol recovery:

- ethanol recovery for alcohol extraction;

- regeneration of low-grade ethanol;

d) water extraction:

- water extraction;

- water washing.

Loading raw materials

It is carried out by pneumatic transport before starting the extraction process. The crushed fraction of vegetable raw materials is used as a feedstock. Loaded raw materials are processed by steam

Extraction with ethanol

It is carried out to extract alcohol-soluble substances and oils from the feedstock. The operation is carried out under vacuum. Ethanol, located in the cube-collector of alcohol-soluble biologically active substances, is heated by hot water supplied to the heat exchanger. Ethanol evaporates, its vapors pass through the sawdust and, condensing on the dephlegmator, flow down through the crushed fractions of the raw material, extracting the biologically active substances. The water-alcohol solution of biologically active substances is periodically drained into the collection cube, which is carried out by switching the positions of the corresponding valves. The design of the installation allows both extraction with hot ethanol vapors and extraction according to the principle of operation of the Soxhlet apparatus (also by switching the positions of the corresponding valves). After extraction with ethanol, the resulting water-alcohol solution of biologically active substances is drained, and the collection cube is again filled with ethanol.

Ethanol recovery

After the implementation of alcohol extraction, part of the ethanol remains in the feedstock. The unit allows this ethanol to be regenerated and returned to the production process. The ethanol regeneration process starts when the solvent is changed from ethanol to water (i.e., when the unit is switched from a collection cube of alcohol-soluble biologically active substances to a collection cube of alcohol-insoluble biologically active substances). The operation is also carried out under vacuum. When distilled water or a water-alcohol solution in a cube-collector of BAS insoluble in alcohol is heated with hot water through a heat exchanger, water vapor displaces ethanol in the raw material, ethanol vapor condenses on a dephlegmator and through a refrigerator enters an alcohol-receiving container, from where, by means of switching the position of the corresponding valve, merge into a cube-collector of alcohol-soluble biologically active substances. Thus, the main part of the ethanol for the next alcohol extraction is returned from the previous extraction.

water extraction

Upon completion of the ethanol regeneration process, the water extraction of BAS insoluble in alcohol is started directly. Distilled water is topped up in the cube-collector of biologically active substances insoluble in alcohol, to the required level, which is then heated with hot water supplied to the heat exchanger. The process is carried out under vacuum. Water evaporates, its vapors pass through the crushed fractions of the raw material and, condensing on the reflux condenser, flow down the fractions, extracting BAS insoluble in alcohol. The aqueous solution of biologically active substances is periodically drained into the collection cube, which is carried out by switching the positions of the corresponding valves. The design of the installation allows both extraction with hot water vapor and extraction according to the principle of operation of the Soxhlet apparatus (also by switching the positions of the corresponding valves). After the aqueous extraction, the resulting aqueous solution of biologically active substances is drained, and the collection cube of BAS insoluble in alcohol is again filled with distilled water or a water-alcohol solution with a low concentration of ethanol (not more than 50%), obtained at subsequent stages of production.

The resulting aqueous extract with a content of BAS insoluble in alcohol, not less than 20%, is sent to spray drying to obtain BAS in the form of a dry powder. The powder is packed in foil bags.

The operation of the reactors in a closed cycle is shown in figures 3 and 4

Thus, the difference lies in a different mode of preparation and contact of raw materials and extractant, in a different design of the device for implementing these changes, i.e. the invention is new.

Claims (2)

1. An installation for the extraction of biologically active substances from a vapor-permeable plant material, consisting of a container for an extractant and an extractor connected by a pipeline, a condensate collector and a receiver, a vacuum pump connected to the receiver, a dephlegmator installed above the extractor, which ensures the condensation of extractant vapors, a heater and a pump, providing heating and supply of heating fluid to the jacket of the container of the extractant and extractor, characterized in that a feature of the installation is the presence of an extractor, a collection cube of alcohol-soluble biologically active substances; cube-collector of alcohol-insoluble biologically active substances; alcohol receiver; refrigerator; dephlegmator; refrigerant supply systems, with the implementation of all processes of extraction, evaporation, concentration, recirculation of the main solvent and drying of the input raw materials in one vat apparatus, using water vapor supplied directly to the extractor and mixed with vapor-permeable raw materials, which significantly speeds up the maceration process and allows substances to be extracted from the solution with one portion of the solvent with more efficient degassing of the raw material. 2. An installation for the extraction of biologically active substances from a vapor-permeable plant material according to claim 1, characterized in that a feature of the installation is the possibility of using convective heat transfer, convective diffusion, to carry out the process of heat propagation in a liquid from the surface of a solid body or to its surface, simultaneously with convection and thermal conductivity, carrying out the distribution of heat, i.e. heat transfer by contact, the use of circulation-type extraction based on the circulation of the extractant, ensuring an effective extraction rate determined by the difference in the concentration of the extractable substance in the liquid that fills the pores of the raw material and in the bulk of the solvent in contact with the surface of the solid particles and diffusion resistance at each stage.

Images