![]() Process for the enrichment of valuable substances from a liquid raw material
专利摘要:
In a process for the enrichment of valuable substances, in particular phytochemicals, such as e.g. Polyphenols, dyes, antioxidants and the like, from a liquid raw material, e.g. Lipids, fermentation broths or solvent extracts, the raw material is mixed in a mixing device (5) with a compressed extractant, in particular CO 2, from a storage container (1), whereupon the mixture is fed to a Vorkonzentratabscheider (13) and the extractant in the higher-soluble components of the undissolved constituents are separated, wherein the loaded extractant from the Vorkonzentratabscheider (13) is withdrawn and the undissolved constituents remain as Vorkonzentrat, wherein the loaded extractant is passed through a separator system in which the dissolved substances are separated from the loaded extractant, wherein the purified extractant the storage container (1) is returned. 公开号:AT513907A1 申请号:T101/2013 申请日:2013-02-07 公开日:2014-08-15 发明作者: 申请人:Natex Prozesstech Gmbh; IPC主号:
专利说明:
• · · · · · · · · · · • 1 · · · ······························· The invention relates to a process for the enrichment of valuable substances, in particular phytochemicals, such as e.g. Polyphenols, dyes, antioxidants and the like, from a liquid raw material, e.g. Lipids, fermentation broths or solvent extracts, as well as an apparatus for carrying out this method. The enrichment of valuable substances from liquids, such as Lipids are of great importance in both the dye and food industries. Also the cosmetics industry and the pharmaceutical industry - in particular the sector for the production of so-called "nutraceuticals" - benefits from the benefits of natural concentrates, colors and flavors. An example of a lipid-containing lipid is paprika oleoresin (also called paprika extract), an extract of red pepper pulp. It contains, among other things, capsanthin and capsorubin, which are responsible for the red color of the pepper fruit. The paprika extract is used in oil- and water-soluble commercial preparations for coloring meat and fish preserves, sweets (marzipan), mayonnaises, sausages and cosmetics. Also as a feed additive for egg yolk and skin pigmentation of poultry fattening, the two dyes are used. The level of dye concentration in various extracts, e.g. Pepper extract is commonly referred to in " Color Units " (CU) - ie color units - measured. High values of color units, therefore, a high concentration of the 2/31 • · • · • ♦ Recyclable materials are preferred in industry, as they have a number of advantages. Higher concentrated recyclables have a much higher stability and durability than recyclables with lower concentrations. One of the reasons for this is that higher-concentrated recyclables have a lower oil content than recyclables with lower concentrations and therefore become less easily rancid. In addition, higher concentrations are advantageous because of their easier incorporation into the desired end products. As a further advantage of highly concentrated recyclables may be mentioned their significantly lower weight, which they have compared with unfinished starting materials, resulting in a further advantage for the use of concentrates results - namely, the significantly lower transport costs. Therefore, a number of processes for the enrichment of valuable substances from liquid raw materials have already been proposed. An example is the multistage, distillative extraction of omega-3 fatty acids from esterified fish oil. Furthermore, it is known, for example, to obtain carotenoid concentrate from algae oil and lycopene concentrate from tomato oil. However, these methods have the disadvantage that the valuable substances are enriched with only low efficiency. Furthermore, a high expenditure on equipment and a high cost to carry out these procedures are necessary. 3/31 ·· ··· ······· ··················································································· · ··· M · J ··· ·· # · · These disadvantages should be avoided. The present invention therefore aims to provide a method and a device which (s) provides the enrichment of a variety of recyclables from liquid starting materials with low equipment and low cost and high efficiency. To achieve this object, the inventive method of the type mentioned is essentially that the liquid raw material is mixed in a mixing device with a compressed extractant, in particular CO2, from a storage container, whereupon the mixture is fed to a Vorkonzentratabscheider and the extractant in the majority easier soluble substances from the undissolved constituents, which include undissolved valuable substances, are separated, wherein the loaded extractant from the Vorkonzentratabscheider is withdrawn and the undissolved constituents remain as Vorkonzentrat, wherein the loaded extractant is passed through a separator system in which the dissolved substances are separated from the loaded extractant and the purified extractant · the storage container is recycled. The extractant is thus used to extract more soluble substances, e.g. short chain lipids are used, so that the less soluble or insoluble substances, e.g. the long-chain lipid constituents, together with the recyclables which are sparingly soluble under the prevailing conditions, remain behind. The economy of the method according to the invention is particularly by the circulation of the 4/31 • MM · »« «* * · · ·················································································································································································································· ·· 'ifM «M · · Extraction agent ensured. Preferably, the extractant is left in the compressed state during the entire cycle, so that complete relaxation and subsequent recompression and the associated effort can be avoided. In principle, the enrichment according to the invention can only take place in one stage, so that the abovementioned preconcentrate represents the end product of the process. Preferably, however, it is provided that the enrichment takes place in two stages, the valuable substances with the slightly soluble constituents of the raw material being concentrated in a first enrichment stage to form a preconcentrate and the preconcentrate being concentrated in a second enrichment stage to form a final concentrate. If necessary, the second enrichment stage is carried out here with changed compared to the first enrichment stage pressure and / or temperature conditions. The two-stage enrichment can be either continuous or discontinuous. The preconcentrate is thus either withdrawn continuously from the Vorkonzentratabscheider and fed to the Vorkonzentratabscheider downstream extractor, in which it is then further concentrated with renewed feed of extractant from the storage tank. The Vorkonzentratabscheider can be designed in this case in the form of a cyclone. Or, according to a further preferred embodiment, the process is further developed such that the preconcentrate in the preconcentrator is enriched further from the storage container to the desired concentration after completion of the feedstock feed with compressed extractant. 5.31 • • • • • • • • * • ♦ * * • • • • • • • • • • • • • • • • V # · - > ♦♦ · ··· »• As an advantage of the continuous process, it can be seen that the preconcentration of the valuable substances in the preconcentrator and their further concentration in the downstream extractor take place at the same time. It is therefore not necessary to wait until the loaded extractant has been withdrawn from the preconcentrator to again feed extractant into the preconcentrator - as is the case in the discontinuous sequence. Parallel to the production of the preconcentrate in Vorkonzentratabscheider can take place in the continuous process namely a renewed feeding of extractant into the downstream extractor and thus the final enrichment of the valuable substances. The process according to the invention is preferably developed further in such a way that the compressed extractant, here called carbon dioxide by way of example, is present in a liquid or supercritical state in the preconcentrator and optionally in the downstream extractor. The advantage of supercritical CO2 over liquid carbon dioxide lies in the fact that the supercritical phase has both a lower viscosity and a lower surface tension than its liquid counterpart. Due to the low viscosity, a high diffusion or by the intensive mixing of the raw material with the supercritical fluid, a rapid mass transfer is achieved. This property thus ensures extraction of soluble in the respective extractant substances from the liquid raw material. 6/31 The process according to the invention is preferably developed such that the pressure in the preconcentrator is chosen such that the more easily soluble substances dissolve more strongly in the extractant than the sparingly soluble valuable substance to be enriched. The pressure in Vorkonzentratabscheider or optionally in the downstream extractor is thus adjusted so that the more soluble substances (eg short-chain lipids) solve, while the poorly soluble fraction (eg long-chain lipids, carotenoids, phytochemicals) in undissolved form in Vorkonzentratabscheider or optionally remains in the downstream extractor. In particular, the pressure should be selected such that the valuable hardly or not at all dissolves. The pressure in Vorkonzentratabscheider or optionally in the downstream extractor is hereby preferably selected between 150 and 450 bar. Particularly preferably, the pressure is between 250 to 400 bar. Advantageously, the method according to the invention is further developed such that the temperature in the preconcentrate separator is selected such that a sufficient difference in density for the separation is achieved. According to the invention the temperature in Vorkonzentratabscheider between 20 and 100 ° C. As a result, a sufficiently low density of the extractant and the substances dissolved therein is achieved which causes the thus loaded extractant in the preconcentrator rises and can be deducted in the sequence. 7.31 The method according to the invention can be developed in particular to the effect that the separation of the dissolved substances from the loaded extractant is favored by a change in the solubility, in particular a pressure and / or a temperature change. Advantageously, the separation of the dissolved substances from the loaded extractant in the process according to the invention can also be effected by adsorption or a membrane process. In particular, it may be provided Hazelnut oil, algae oil, crustacean oil, paprika oleoresin, rice peel oil, coffee oil, fatty acid distillate, fermentation broths or toasted aromatic oil as liquid raw material for subsequent enrichment of the valuable substances contained therein and accordingly lycopene, hazelnut flavor, carotenoids, colorings, nutraceuticals, coffee flavors, tocopherol or toasted flavors concentrate concentrated valuable material. The process according to the invention is advantageously developed in such a way that the final concentrate is discharged via a final concentrate separator in which the extractant remaining in the final concentrate is separated off. This step ensures further separation of the extractant remaining in the stock concentrate, with the result that the end product of the claimed process is in a much purer form than without this last step and that a higher level of extractant can be recycled to the storage container. 8/31 ·· ···· The apparatus for carrying out the method described above comprises a compressed extractant storage container, a liquid raw material storage container, a mixing device connected to the compressed extractant storage container and the liquid raw material storage container, a separator connected to the mixing apparatus , which has a discharge port for discharging a loaded extractant and a discharge port for discharging a preconcentrate, the discharge ports for discharging the loaded extractant being connected to a separator system connected to the compressed extractant storage container through a return line. For intensive mixing of the extractant with the liquid raw materials, the inventive construction can be developed such that the mixing device is designed as a static mixer, mixing chamber or nozzle. In order to ensure the extraction of media which are difficult to extract and / or those having a solids content, the formation according to the invention may further preferably be such that the downstream extractor is designed as a thin-layer extractor or as a column extractor. A thin-layer extractor is to be understood as meaning a device as can be taken, for example, from WO 2004/018070 A1. Such a thin-layer extractor has a pressure-resistant reactor with at least one feed opening for the pre-extract and the compressed extractant to be treated, and corresponding 9/31 · Q Q · · · · · · · · Discharge openings, wherein the feed opening for the pretreatment to be treated opens on the inner jacket of the reactor, at which forms a film-like layer of the pre-extract. Inside the reactor, a rotor is arranged, the radial arms of which interact with the preconcentrate film on the inner jacket of the reactor. By the use of a reactor, inside which a rotor is arranged, the possibility is created to make the mechanical action by additional action of centrifugal forces, whereby a correspondingly rapid rotation for applying the desired centrifugal force can take place. At the same time, the rotor forms the tools for machining the thin film, which in the simplest case can be formed by wipers, rollers, doctor blades or the like. The thickness of the film is determined by the preset distance of the rotating tool to the inner jacket of the reactor. The tools, such as Rolls may have a helical profiling, but may also be conical, concave or convex, wherein the profiling during unwinding along the preconcentrate film simultaneously promotes downward movement of the film in the direction of the discharge opening. In countercurrent to the pre-concentrate now the extractant is introduced into the reactor, wherein the corresponding feed opening is formed in the bottom part. The extractant rises in the interior of the reactor and comes into intensive contact with the preconcentrate film, wherein the surface of the film exposed to the extractant is constantly renewed by the kneading process effected by the rotating tools. The loaded extractant · can be withdrawn in the sequence via an outlet opening provided in the lid. 10/31 • · * * · · · ·································································································. * ···· «••• l '* ·····» * The device according to the invention is developed in an advantageous manner to the effect that the discharge of Vorkonzentratabscheiders for dispensing the preconcentrate with a downstream extractor is in communication and that in the Vorkonzentratabscheider connecting to the downstream extractor line another mixing device is arranged, which is connected to the storage container , This further mixing device allows an additional separation of dissolved in the extractant substances and thus favors the recovery of a final product with very high purity. According to the invention, the device can be designed such that additional extractors are arranged after the previously mentioned extractor for further concentration, wherein the feed takes place in each case via a mixing device in which fresh extractant and correspondingly preconcentrated valuable material mixture from the respective previous extractor are intensively mixed. Advantageously, the device is further developed in that the separator system comprises at least two separators, which are connected to each other with the interposition of at least one throttle valve. This ensures that different pressures prevail in the various separators of the system, which are chosen to be lower than the pressure in Vorkonzentratabscheider, which causes the substances dissolved in the extractant can be separated again from the extractant and that the purified 11/31 Extraction agent can be recycled to the storage container. Preferably, the device is designed such that a discharge opening of Vorkonzentratabscheiders or the downstream extractor for dispensing the pre- or final concentrate is connected to a Endkonzentratabscheider whose discharge is connected to the recovery of the remaining extractant via a line and a downstream compressor to the storage container. The invention is described below with reference to Embodiments explained in more detail. In the following process examples, a two-stage enrichment of recyclables is described in each case. In this case, the second enrichment step is carried out after completion of the first enrichment step, so that it is a total of a discontinuous procedure. Example No. Step # 5463 g of paprika oleoresin (30070CU) was injected at a mass flow rate of 9.2 g / min radially to supercritical CO2 (350 bar, 50 ° C) into a mixer formed by a tube. The mass flow of CO2 was 33kg / h. The mixture of loaded CO2 and the CO2-undissolved portion of the oleoresin in the mixing device was led to a preconcentrate separator in which the loaded CO2 was separated from the undissolved in CO2 portion of the oleoresin. The loaded CO2 became 12/31 • »· · · · · · · · · · · · · · · · · · · · · · · ··································································································································································· The undissolved portion of the oleoresin was accumulated in the preconcentrate separator. After 600 minutes, 4211 g of paprika extract (dye value 10035CU) were withdrawn from the preconcentrate separator with the loaded CO2 and can be utilized as a by-product. The im Preconcentrate accumulated residue weighed 1252g and had a dye level of 59700CU. Step # 2 1252g of the preconcentrate obtained in Step 1 (paprika oleoresin having a color value of 59760CU) were charged to an extractor. The extractor used in this case may be the preconcentrate separator used in step 1 or a separate aggregate. The preconcentrate was extracted with supercritical CO2 at 33kg / h at 350bar and 50 ° C. After about 150 minutes or 83 kg of CO2, 548 g of oleoresin extract (dye value 10420CU) were removed from the extractor with the loaded CO2. The remaining residue (704 g) in the extractor reached a colorant value of 104000CU. Example No. 2 Step # 3542g of paprika oleoresin (30070CU) was injected at a mass flow rate of 9.2 g / min radially to supercritical CO 2 (350 bar, 50 ° C) in a mixer formed by a tube. The mass flow rate of CO 2 was 33kg / h. The mixture of charged CO 2 and CO 2 undissolved portion of the oleoresin formed in the mixing device was conducted to a preconcentrate separator in which the charged CO 2 was removed from the undissolved CO 2 in the CO 2. · · · · · · · · · · · · · · · · Proportion of oleoresin was separated. The loaded CO2 was further expanded into a separator system. The undissolved portion of the oleoresin was accumulated in the preconcentrate separator. After 385 minutes, 2505 g of paprika extract (dye value 10060CU) were withdrawn from the preconcentrate separator with the loaded CO2 and can be utilized as a by-product. The im Preconcentrate accumulated residue weighed 1037g and had a dye level of 58852CU. Step # 2 1037 g of the preconcentrate obtained in step 1 (paprika oleoresin having a color value of 59760CU) were placed in an extractor. The extractor used in this case may be the preconcentrate separator used in step 1 or a separate aggregate. The preconcentrate was extracted with supercritical CO2 at 33kg / h at 350bar and 50 ° C. After about 135 minutes or 75 kg of CO2, 485 g of oleoresin extract (dye value 10082CU) were removed from the extractor with the loaded CO2. The remaining residue (552 g) in the extractor reached a colorant value of 105348CU. The device according to the invention will be explained in more detail with reference to embodiments schematically illustrated in the drawing. 1 shows a device for the batch process according to the present invention, and FIG. 2 shows a device for the continuous process according to the present invention. In Fig. 1, a storage container for the compressed extractant is denoted by 1 and a storage container for the liquid raw material is denoted by 2 for the liquid raw material. The storage containers 1 and 2 are connected via the lines 3 and 4 with the mixing device 5. In line 3, the extractant is compressed by the use of the motor-driven pump 7 and thereby brought to the desired pressure level. To avoid cavitation in pump 7 either a pre-pressure pump 6 or a pre-cooler in line 3 is installed. In addition, the heat exchanger 8 brings the compressed extractant to the desired temperature. Similarly, the heat exchanger 9, which is located in line 4, provides for adjusting the temperature of the liquid raw materials. The flow of the compressed extractant and the liquid raw materials can be controlled by means of speed regulators on the pumps 7 and 12. Since the solution process is dependent on the amount of extractant, the ratio of liquid raw material to volume flow of the extractant influences the extraction performance and can be adjusted individually by the speed controls of the pumps 7 and 12. The guided through the shut-off valve 10 liquid raw material is fed by means of the downstream pump 12 in the mixing device 5, while the compressed extractant reaches the mixing device 5 via line 3. In the mixing device 5, which is preferably designed as a static mixer, the two components are mixed intensively. This results in a disperse mixture of extractant and liquid raw material. This mixture is withdrawn from the mixing device 5 and spent in the Vorkonzentratabscheider 13. in the Preconcentrate separator 13 prevails e.g. a pressure of 350 bar at a temperature of e.g. 50 ° C. Here are the more easily soluble components such as the short-chain 15/31 • 15. • ♦ • • Μ • · Lipids in dissolved form in the extractant, while the fraction of sparingly soluble components such as e.g. the long-chain lipids and valuable substances are undissolved in Vorkonzentratabscheider 13. The density difference of the two fractions leads to the formation of two phases - in the extractant - the more readily soluble components such as short chain lipids as the first phase and undissolved sparingly soluble components such. long-chain lipids and valuable substances as the second phase. The first of the above-described loaded phases subsequently rises due to their lower density upwards and is withdrawn there via the discharge opening 14. The selected pressure and temperature level ensures a sufficient density difference between the two phases. In Vorkonzentratabscheider 13, a corresponding distribution system is installed. The discharge opening 14 is connected via the line 15 to a separator system which consists of two separators 16 and 17 arranged downstream of the preconcentrator. The line 15 further has a throttle valve 18 which controls the extractant flow as needed. The respective pressure level in the downstream separators 16 and 17 is gradually reduced, the separator 16 having an internal pressure of for example 90-120 bar and the separator 17 having an internal pressure of, for example, only 40-60 bar. The two separators 16 and 17 are connected to each other via the line 19, wherein the pressure of the loaded extractant in separator 16 is regulated by a further throttle valve 20 and via the heat exchanger 21, an increase in the temperature and / or evaporation of the extractant is achieved. About the 16/31 »· # ··· 1 & · · · ··· * ♦ Lines 22 and 23 can therefore by means of the control valves 24 and 25, the poorly soluble components deposited by the extractant such as. Triglycerides and recyclables are withdrawn, wherein the now unloaded extractant via line 35 and with the interposition of a capacitor 27 again the storage container 1 is supplied. The extracting agent reaching the storage container 1 thus already has the correct temperature and the correct pressure again at this time in order to be fed back to the process. To enrich the desired recyclables, the remaining after completion of the feed of liquid raw material in the Vorkonzentratabscheider 13 undissolved fraction of recyclables (the preconcentrate) via the discharge port 26 - or optionally brought by renewed supply of compressed extractant from line 3 to the desired concentration , The concentrate thus obtained is thus introduced into the line 28 and reaches the final concentrate separator 29, from which the final concentrate is subsequently transported via the discharge opening 30 in line 31, wherein the withdrawal can be controlled via a control valve 32. The pressure in Endkonzentratabscheider 29 is adjusted by means of a control valve 50. In the discontinuous process there is thus a pressure difference between the pre-concentrate separator 13 and the final concentrate separator 29, which makes it possible to extract the liberated extractant via the further discharge opening 33 and by means of the 17 motor driven compressor 34 via the line 35 and the capacitor 27 in to recycle the storage container 1. Fig. 2 describes the continuous flow of the method according to the invention. The steps carried out essentially correspond to those of the batch process (see Fig.l). However, in addition to the process described in FIG. 1, the continuous process includes a further conduit 36 in which the extractant is compressed by the use of the motor-driven pump 38 and brought to the desired pressure level. To avoid cavitation in pump 38 either a pre-pressure pump 37 or a pre-cooler in line 36 is installed. Furthermore, the heat exchanger 39 ensures that the compressed extractant to bring to the desired temperature. In addition, the continuous process includes an extractor 40 connected downstream of the preconcentrator 13 and a further mixing device 41 arranged between preconcentrator 13 and downstream extractor 40. The amount withdrawn from the preconcentrator 13 via line 28 can be measured via a fill level measurement in the preconcentrator 13 and / or a corresponding pump 51 be managed. The discharge opening 26 together with line 28 and the line 36 open into the mixing device 41, where a renewed intensive mixing of the withdrawn from the Vorkonzentratabscheider 13 preconcentrate and the extraction agent from line 36 takes place. The mixture thus obtained is fed in the sequence in the downstream extractor 40. In the downstream extractor 40, there is either the same pressure as in the upstream 18/31 ···························································································. * 1Q · · · · ♦ · · · IO · * ····· ··· ··· tt »» · Preconcentrate separator 13 - e.g. 350 bar, or depending on the solubility of the additional components to be removed, a predominantly increased pressure. The less soluble components thus dissolve in the extractant while the fraction of recyclables and higher polar components remain undissolved in the downstream extractor 40. The density difference of the two fractions leads, as already described above, to the formation of two phases. The first phase loaded with the additional components to be removed increases and is withdrawn via the further discharge opening 49 from the downstream extractor 40. In order to obtain the concentrate of desired recyclables, the remaining in the downstream extractor 40 unresolved fraction of recyclables and higher polar components is withdrawn via the discharge port 42 and spent in the line 43, this can be regulated again via a throttle valve 44 and then reaches the End Konzentratabscheider 45, which with eg 10 bar internal pressure has a substantially lower pressure than the extractor 40. The final concentrate is withdrawn via line 46 from the Endkonzentratabscheider 45, this being again regulated via a throttle valve 47, while any remaining amount of extractant via the discharge opening 48 into the storage container. 1 is returned. 19/31
权利要求:
Claims (19) [1] ··· * ·· Claims 1. A process for the enrichment of valuable substances, in particular phytochemicals, such as, for example, Polyphenols, dyes, antioxidants and the like, from a liquid raw material, e.g. Lipids, fermentation broths or solvent extracts, characterized in that the raw material is mixed in a mixing device (5) with a compressed extractant, in particular CO 2, from a storage container (1), whereupon the mixture is fed to a Vorkonzentratabscheider (13) and higher in the extractant soluble components from the undissolved constituents which include the undissolved recyclables are separated, wherein the loaded extractant from the Vorkonzentratabscheider (13) is withdrawn and the undissolved constituents remain as pre-concentrate, wherein the loaded extractant is passed through a separator system in which the dissolved Substances are separated from the loaded extractant, wherein the purified extractant is returned to the storage container (1). [2] 2. The method according to claim 1, characterized in that the preconcentrate is continuously withdrawn from the Vorkonzentratabscheider (13) and fed to the Vorkonzentratabscheider (13) downstream extractor (40), in which it under feeding of extractant from the storage container (1) on is concentrated to obtain a final concentrate. [3] 3. The method according to claim 1, characterized in that the preconcentrate in Vorkonzentratabscheider (13) after 20/31 ♦ ♦ ◆ ··············································· compressed extractant from the storage container (1) is further enriched to the desired concentration to obtain a final concentrate. [4] 4. The method according to any one of claims 1 to 3, characterized in that the mixing device (5,41) is designed as a static mixer, mixing chamber or nozzle. [5] 5. The method according to any one of claims 1 to 4, characterized in that the compressed extractant in liquid or supercritical state in Vorkonzentratabscheider (13) and optionally in the downstream extractor (40) is present. [6] 6. The method according to any one of claims 1 to 5, characterized in that the pressure in Vorkonzentratabscheider (13) is selected such that the more soluble components in the extractant solve more than the valuable material to be enriched, the pressure 150 to 450 bar, in particular 250 to 400 bar. [7] 7. The method according to any one of claims 1 to 6, characterized in that the temperature in Vorkonzentratabscheider (13) is selected such that sufficient for the separation density difference is achieved, wherein the temperature is between 20 and 100 ° C. [8] 8. The method according to any one of claims 2 to 7, characterized in that the downstream extractor (40) is designed as a thin-layer extractor or as a column extractor. 21/31 ·· •··········································································································································································································· [9] 9. The method according to any one of claims 1 to 8, characterized in that a plurality of the Vorkonzentratabscheider (13) downstream extractors is provided, which are arranged in series, each extractor of the preceding in the row each extractor and fresh extractant fed becomes. [10] 10. The method according to claim 9, characterized in that the extraction is carried out in the downstream or the extractor (s) with changed compared to the preceding extractor pressure and / or temperature conditions. [11] 11. The method according to any one of claims 1 to 10, characterized in that the separation of the dissolved substances from the loaded extractant comprises a change in the solubility, in particular a pressure and / or a temperature change. [12] 12. The method according to any one of claims 1 to 10, characterized in that the separation of the dissolved substances from the loaded extractant comprises an adsorption or a membrane process. [13] 13. The method according to any one of claims 1 to 12, characterized in that as raw material tomato oil, hazelnut oil, algae oil, crustacean oil, paprika oleoresin, rice shell oil, coffee oil, fatty acid distillate or roasted, aromatic oil is used. [14] 14. The method according to any one of claims 1 to 13, characterized in that as valuable material lycopene, hazelnut flavor, 22/31 · ♦ ··· ♦ 2 · · · · δ ·· φ ···· · carotenoids, dyes, nutraceuticals , Coffee flavors, tocopherol or toasted flavors are selected. [15] 15. The method according to any one of claims 1 to 14, characterized in that the final concentrate via a Endkonzentratabscheider (29,45) is discharged, is separated in the remaining in the final concentrate extractant. [16] 16. A device for carrying out the method according to any one of claims 1 to 15, comprising a storage container (1) for a compressed extractant, a storage container (2) for liquid raw material, a mixing device (5) to the storage container (1) for the compressed extractant and connected to the liquid raw material storage tank (2), a preconcentrator (13) connected to the mixing device (5) having a discharge port (14) for discharging a loaded extractant and a discharge port (26) for discharging a preconcentrate wherein the discharge openings (14) for discharging the loaded extractant is connected to a separator system, which is connected via a return line (35) to the storage vessel (1) for the compressed extractant. [17] 17. An apparatus for carrying out the method according to claim 16, characterized in that the discharge opening (26) for discharging the preconcentrate with a downstream extractor (40) is in communication and in the Vorkonzentratabscheider (13) with the downstream extractor (40) connecting Line (28) a further mixing device (41) is arranged over 23/31 ·· • · · * * * t · · another line (36) is connected to the storage container (1). [18] 18. Device according to one of claims 16 or 17, characterized in that the separator system comprises at least two separators (16,17) which are interconnected with the interposition of at least one throttle valve (20). [19] 19. The device according to any one of claims 16 to 18, characterized in that a discharge opening (26,42) of the Vorkonzentratabscheiders (13) or the downstream extractor (40) for dispensing the pre-or final concentrate with a Endkonzentratabscheider (29,45) is connected, the discharge opening (33,48) for discharging the remaining extractant via a line (35) and a downstream compressor (34) to the storage container (1) is connected. Vienna, February 7, 2013 Applicants by: 24/31
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同族专利:
公开号 | 公开日 WO2014121311A1|2014-08-14| MX2015010196A|2016-04-28| AT513907B1|2015-01-15| EP2953699A1|2015-12-16|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 DE3810681A1|1988-03-29|1989-10-12|Udo Kienle|METHOD FOR PRODUCING A NATURAL SWEETENER BASED ON STEVIA REBAUDIANA AND ITS USE| DE4306303A1|1993-03-01|1994-09-08|Barth Raiser Hopfenextraktion|Process for obtaining vegetable oils by extraction| DE4335321A1|1993-10-15|1995-04-20|Joachim Brimmer Ingenieurbuero|Process for extracting coffee oil-containing aroma constituents| WO2004018070A1|2002-08-26|2004-03-04|Natex Prozesstechnologie Gesmbh|Method and device for the extraction of materials from liquids or solid dispersions| WO2006131378A2|2005-06-08|2006-12-14|Terra Nostra Produkte Mit Naturextrakten Gmbh|Method for producing margosa extract| US20080260852A1|2007-01-23|2008-10-23|Ferro Pfanstiehl Laboratories, Inc.|Supercritical fluid extraction produced by in-line homogenization|CN111921228A|2020-07-29|2020-11-13|周民主|Ultrasonic reinforced supercritical fluid extraction method|GB769454A|1953-08-24|1957-03-06|Herbert Peter August Groll|Fractionation of oils or other soluble mixtures of organic substances by selective extraction| US4770780A|1984-04-25|1988-09-13|Cf Systems Corporation|Liquid CO2 /cosolvent extraction| JPS61268762A|1985-05-24|1986-11-28|Mitsubishi Kakoki Kaisha Ltd|Concentration of naturally-occurring dyestuff| DE69723294T2|1996-12-06|2004-05-27|Advanced Phytonics Ltd.|MATERIALS TREATMENT| CN1280025A|2000-08-14|2001-01-17|孙传经|Multifunctional-supercritical CO2 extraction technology| US6589422B2|2000-12-18|2003-07-08|Ineos Fluor Holdings Limited|Apparatus and method for extracting biomass|CN104927665B|2015-05-20|2017-06-16|山东天博食品配料有限公司|A kind of method that utilization supercritical carbon dioxide extracting fermented capsicum prepares capsicum oleoresin|
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申请号 | 申请日 | 专利标题 ATA101/2013A|AT513907B1|2013-02-07|2013-02-07|Process for the enrichment of valuable substances from a liquid raw material|ATA101/2013A| AT513907B1|2013-02-07|2013-02-07|Process for the enrichment of valuable substances from a liquid raw material| PCT/AT2014/000006| WO2014121311A1|2013-02-07|2014-01-14|Method for enriching valuable substances from a liquid raw material| EP14705694.9A| EP2953699A1|2013-02-07|2014-01-14|Method for enriching valuable substances from a liquid raw material| MX2015010196A| MX2015010196A|2013-02-07|2014-01-14|Method for enriching valuable substances from a liquid raw material.| 相关专利
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